Synthesis, Crystal Structure and Properties of 2,7-Bis [4-（diphenylamino）phenyl] fluorene

A novel fluorene derivative containing triphenylamine groups, 2,7-bis[4-(diphenylamino)-phenyl]fluorene (C49H36N2 , Mr= 652.80), was synthesized via Suzuki coupling reaction (yield: 19%) and its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 9.320(4), b = 11.250(6), c = 17.369(6) , α = 88.035(3), β = 86.450(5), γ = 73.524(5)°, V = 1742.8(13) 3 , Z = 2, Dc = 1.244 g/cm 3 , μ(MoKα) = 0.072 mm -1 , F(000) = 688, S = 1.095, the final R = 0.0616 and wR = 0.1878. It presents a linear framework constituted by a linkage of fluorene as a bridge and two triphenylamine groups. Its spectral and electrochemical properties were studied by UV-Vis absorption, fluorescence spectroscopy and cyclic voltammetry (CV). This compound can emit intense blue fluorescence with a peak wavelength of 446 nm and a full width at half maximum (FWHM) of 38 nm under UV excitation at 350 nm in film. The highest occupied molecular orbital (HOMO) energy level, the lowest unoccupied molecular orbital (LUMO) energy level and optical band gap (Eg) of the title compound are -5.46, -2.57 and 2.89 eV, respectively.     

Synthesis,Crystal Structure and Biological Activity of 2-Chloro-N-{2-fluoro-5-[N-（phenylsulfonyl） phenyl-sulfonamido]phenyl}benzamide

2-Chloro-N-{2-fluoro-5-[N-（phenylsulfonyl）phenylsulfonamido]phenyl}benzamide was synthesized and its crystal structure was also determined by X-ray single-crystal diffraction. The title compound（C25H18ClFN2O5S2） belongs to monoclinic, space group P21/n with a=0.7377（3） nm, b=1.2036（5） nm, c=2.6846（11） nm, β=90.895（9）°, V=2.3833（16） nm3, Mr=544.98, Z=4, Dc=1.519 g/cm3, μ=0.385 mm–1, F（000）=1120, R1=0.0632, and wR2=0.1438. Its crystal structure belongs to a novel class that has not been reported yet, and its preliminary herbicidal activity was also tested. Its inhibition rate to seedling growth of barnyard grass reaches 15.1% at 100 μg/mL.     

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 [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 and Crystal Structure of N-（2-（1,3,4-oxadiazol-2-yl）phenyl）-2,3-dimethylaniline

The title compound, N-（2-（1,3,4-oxadiazol-2-yl）phenyl）-2,3-dimethylaniline, was synthesized and studied by single-crystal X-ray diffraction method. The structure of the product was confirmed by IR, ^1H- and ^13C-NMR spectroscopy, elemental analysis and mass spectrometry. These experimental studies were supported by theoretical optimizations.     

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 and Crystal Structure of N-[2-（4-Chlorophenyl）-1-（1-methylcarbamoyl-2-phenyl-ethylcarbamoyl）-3-phenyl-cyclopropyl]-benzamide

N-[2-(4-chlorophenyl)-1-(1-methylcarbamoyl-2-phenyl-ethylcarbamoyl)-3-phenyl-cyclopropyl]benzamide,C33H30ClN3O3,has been synthesized and characterized by IR,1H NMR,13C NMR and single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 11.646(2),b = 13.795(3),c = 14.559(3),α = 76.422(4),β = 78.028(4),γ = 74.500(4)°,V = 2164.6(7)3,Z = 3,Mr = 552.05,Dc = 1.270 g/cm3,λ = 0.71073 ,μ(MoKα)= 0.171 mm–1,F(000)= 870,the final R = 0.0469 and wR = 0.0805 for 5554 observed reflections with I > 2σ(I).The N–H and oxygen atoms are involved in one-dimensional intermolecular hydrogen bonds,which further stabilize the structure.     

Synthesis and Crystal Structure of 4-Chloro-N- （2-（2-nitrophenyl）acetoxy）-N-（m-tolyl）benzamide

The new title compound 4-chloro-N-(2-(2-nitrophenyl)acetoxy)-N-(m-tolyl)benzamide(C22H17ClN2O5, Mr = 424.82) has been synthesized via the reaction of 4-chloro-N-hydroxy-N-(m-tolyl)benzamide with 2-(2-nitrophenyl)acetyl chloride. The structure of the product was confirmed by 1H NMR, 13 C NMR, IR, HRMS(ESI) and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a = 13.0269(10), b = 6.7251(6), c = 23.9313(16) , β = 99.931(6)o, V = 2065.1(3) 3, Z = 4, Dc = 1.366 g/cm3, F(000) = 880, μ = 0.221 mm-1, the final R = 0.0600 and wR = 0.1754 for 1981 observed reflections(I 2σ(I)). X-ray analysis indicates that the chloro-phenyl ring(C(10)~C(15)) and the methyl-substituted benzene ring(C(16)~C(21)) are not coplanar with the nitro-substituted benzene ring(C(1)~C(6)), with the dihedral angle to be 70.78° and 63.72°, respectively. Hydrogen bonds C(2)–H(2)···O(2) and C(7)–H(7B)···O(5) are observed.     

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.     

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.     

Synthesis,Crystal Structure,Characterizationand Quantum Chemical Studies on 1N-Acetyl-3-（2,4-dichloro-5-fluorophenyl）-5-（p-methyl-phenyl）-2-pyrazoline

1N-Acetyl-3-（2,4-dichloro-5-fluoro-phenyl）-5-（p-methyl-phenyl）-2-pyrazoline has been synthesized and characterized by elemental analysis, IR, UV-Vis and X-ray single-crystal diffraction. Ab intio calculations have been carded out for the compound by using both B3LYP and HF methods at the 6-31G^＊ basis set. The calculated results show that the predicted geometry can well reproduce the structural parameters. The electronic absorption spectra calculated by B3LYP/6-31G^＊ method are approximate to the experiments and the Natural Bond Orbital （NBO） analyses suggest that the above electronic transitions are mainly assigned to n→π^＊ and π→π^＊ transitions. CIS-HF/6-31G^＊ method is not suitable to predict the electronic spectra for the title compound. The calculation of the second order optical nonlinearity was carded out, giving the value of molecular hyperpolarizability equal to 2.194^＋ 10^-30 esu. On the basis of vibrational analyses, the thermodynamic properties of the compound at different temperature have been calculated, revealing the correlation between C p, m^0, S m^0, H m^0 and temperature.     

Crystal Structure and Antitumor Activity of Tri[2- [N-(4''''-methyl-benzylsulfonyl)amino]ethyl]-amine

1 INTRODUCTION The supramolecular architectures of tripodal ligands with special cavities have attracted much attention of chemists and biochemists because of their interesting structures and possible properties such as ion and molecular recognition, selective inclusion and important biological function[1～5]. However, their potential applications in supra- molecular and biological chemistry for constructing various complexes have not been clearly realized until recent years. Few crystal…     

Synthesis and Crystal Structure of Bis-{N-[2-(6-ethylpyridyl)]-salicylideneiminato} Cobalt(Ⅱ)

1 INTRODUCTION The Schiff bases derived from salicylaldehyde and 2-aminopyridine derivatives have been used as potentially terdentate ligands[1]. Yamada and Yam- anouchi have synthesized the type of ML2nH2O complexes (M = CoⅡ, NiⅡ, CuⅡ, ZnⅡ or PdⅡ)[     

新磺酰脲类化合物N-[2-(4-甲基)嘧啶基]-N''''-2-甲氧羰基苯磺酰脲的合成及其二聚体结构

合成并用X-射线晶体衍射法测定了标题化合物 (C14H14N4O5S, Mr = 350.35)的结构。晶体属正交晶系, 空间群为Pna21, 晶胞参数a = 13.242(4), b = 9.478(3), c = 24.889(8) ? V = 3123.7(17) 3, Z = 8, Dc = 1.490 g/cm3, m = 0.241 mm-1, F(000) = 1456。独立可观测点数为3268。最终偏离因子R = 0.0592, wR = 0.1217 (I > 2s(I) 2153), S = 1.122。X-射线衍射证实标题化合物分子晶体中存在2种构型, 分子中苯环所在的位置同嘧啶磺酰脲平面的取向相反。每种构型中嘧啶磺酰脲、苯环及甲氧羰基分别形成3个独立的平面共轭体系。除此之外, 经由O(1)N(6)和N(2)O(6)形成的分子间氢键以及苯环平面间的p-p 相互作用将2个分子结合在一起从而形成二聚结构。     

Crystal Structure and Antitumor Activity of Tri[2-[N-（4′-methyl-benzylsulfonyl）amino]ethyl]-amine

The crystal structure of the title compound (C27H38N4O7S3, Mr = 626.79) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pīwith a = 9.411(1), b = 11.645(2), c = 14.672(2) (A。), α = 91.80(1), β = 95.36(1), γ =104.56(1)o, V = 1547.0 (A。)3, Z = 2, Dc = 1.346 g/cm3, λ = 0.71073 (A。), μ(MoKα) = 0.289 mm－1 and F(000) = 664. The structure was refined to R = 0.0406 and wR = 0.1177 for 4103 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the title compound is a practically distorted tetrahedron and each molecule contains one lattice H2O by hydrogen bond. The antitumor activity of the title compound against HL-60 human leukemia cells has also been studied by MTT method.     

具有生物活性的N-苯基-N'-(1,3-噻唑-2-基)-1,2,3-苯并噻二唑-7-甲脒的 晶体结构与理论计算

本文设计合成了一种新的植物激活剂先导化合物的衍生物N-苯基-N′-(1,3-噻唑-2-基)-1,2,3-苯并噻二唑-7-甲脒,并进行了元素分析、1HNMR、IR和MS测定。采用密度泛函理论在B3LYP/6-311 +G*水平上对该化合物进行了分子几何结构全优化和频率计算,计算表明,该分子结构中存在N－H···N分子内氢键,从而使分子更加稳定;计算结果还得到分子的红外与拉曼光谱以及不同溶剂相下的电子吸收光谱和不同温度下的热力学性质,为该类化合物构效关系的研究奠定了基础。     

3-[3-甲氧基-4-(2-乙氧基-2-氧代乙氧基)苯基]丙烯酸乙酯的合成及其晶体结构

以香草醛为原料,经Williamsom反应和Knoevenagel-Doebner反应制得新化合物3-(3-甲氧基-4-羧甲氧基苯基)丙烯酸(2);2与乙醇经酯化反应合成了阿魏酸衍生物——3-[3-甲氧基-4-(2-乙氧基-2-氧代乙氧基)苯基]丙烯酸乙酯(3),其结构经1H NMR,IR,元素分析和X-射线单晶衍射确证。3属三斜晶系,空间群P-1,晶胞参数a=8.301,b=8.474,c=11.445,α=82.94°,β=86.86°,γ=84.52°,V=794.63,Z=2,Dc=1.289 g·cm-3,R1=0.046 7,wR2=0.101 8。3通过分子间氢键(C-H┈O)形成了二维网状结构。     

Synthesis and Crystal Structure of N-[1-(4-Chlorophenyl)- 1,4-dihydro-4-oxe-6-methylpyridazine-3-carbonyl]- N'-benzoylhydrazine

1 INTRODUCTION Pyridazinone derivatives represent one of the most active classes of compounds possessing a wide spectrum of biological activity. It was widely used in pharmaceuticals and agrochemicals[1, 2]. Rohm Haas Company had reported that pyridazinones exhibit useful plant growth regulating effects [3,4]. It was also reported that diacylhydrazines exhibit excellent insecticides [5~7]. In view of these facts, it was contemplated to synthesize compounds con- taining both pyridazinone …