含萘环骨架液晶化合物的合成

含萘环骨架液晶化合物的合成;液晶;萘环;合成;熔点;清亮点;液晶相区间     

新型含氮配体钴配合物的水热合成、晶体结构及荧光性质

以4,5-二羟基苯-1,3-二磺酸钠（Na₂H₂L）和4,4′-bipy为原料,采用水热法与Co(NO₃)₂反应合成了新的含氮配体钴配合物[Co(4,4′-bipy)(H₂O)₄]·H₂L·2H₂O（1）（H₂L^2-=4,5-二羟基苯-1,3-二磺酸根离子,4,4′-bipy=4,4′-联吡啶）,其结构和组成经X-射线单晶衍射、红外光谱、元素分析和热重分析表征。晶体结构解析表明：钴离子与4,4′-bipy和水分子配位,形成扭曲的八面体配位构型。H₂L^2-配体没有配位,仅起平衡电荷作用。在结构单元中,[Co(4,4′-bipy)(H₂O)₄]²⁺, H₂L^2-和自由水分子之间通过氢键相连。配合物的荧光发射峰与配体相比发生了蓝移,最大发射峰位于357 nm。     

Reactions of p-Nitrophenyloxirane with Amines Containing Fragments with Bicyclic Skeleton

Reactions of p-nitrophenyloxirane with amines containing fragments with bicyclic skeleton of norbornene, norbornane, epoxynorbornane (stereoisomeric exo- and endo-5-aminomethylbicyclo[2.2.1]hept-2-enes, N-benzyl-endo-5-aminomethylbicyclo[2.2.1]hept-2-ene, endo-5-(2-aminoethyl)bicyclo[2.2.1]hept-2-ene, stereoisomeric exo- and endo-2-aminomethylbicyclo[2.2.1]heptanes, 2-(1-aminoethyl)bicyclo[2.2.1]heptane, exo-5-aminomethyl-exo-2,3-epoxybicyclo[2.2.1]heptane) were investigated. The aminolysis of p-nitrophenyloxirane occurred regioselectively according to Krasusky rule as was proved by ¹H and ¹³C NMR data. As shown by ¹H and ¹³C NMR spectroscopy the oxyalkylation product obtained from N-benzyl-endo-5-aminomethylbicyclo[2.2.1]hept-2-ene was composed of two diastereomers originating from the presence of a chiral nitrogen atom in the rear part of the rigid bicyclic skeleton. New products of amino groups transformation in the molecules of hydroxyamines were obtained by reaction with p-methylbenzoyl chloride and p-nitrophenylsulfonyl chloride. Regioselectivity of the attack of electrophilic reagents on the nitrogen in the hydroxyamines was confirmed by IR and ¹H NMR spectra of the products. The data on pharmacological activity tests of N-2-hydroxyethyl(p-nitrophenyl)-5-aminomethylbicyclo[2.2.1]hept-2-ene are reported.     

Synthesis and Crystal Structure of a New Class of Oxygen Bridged Bicyclic Tetraphosphazanes

Abstract

The reaction of primary amine hydrochlorides with phosphorus oxychloride in the presence of 1/4 mole of H₂0 yields the title compounds I (R = C₆H₅-, 4-CH₃CH₆H₄ ^?′ 4-CH₃CH₆H₄ ^?, 3-CH₃CH₆H₄ ^? CF₃CH₂-). Hydrochlorides Of more basic amines do not yield any cyclic material. The compound I (R = C₆H₅) was isolated as one isomer. An X-ray crystallographic study has shown an open ring structure in which the two chlorine atoms are positioned on the same face of the P₄N₄ ring as the P-O-P bridge.     

Alkynyl-modified Naphthalimide： Synthesis, Crystal Structure and Fluorescence Spectrum

A novel alkynyl substituted N-aryl-1,8-naphthalimide II （C20H11NO2） was synthesized for the discovery and evaluation of new fluorescence probes, and was characterized by X-ray crystal diffraction. It crystallizes in monoclinic, space group P21/n with a = 15.898（3）, b = 5.0102（10）, c = 17.962（4）A, β = 92.97（3）°, V = 1428.7（5） A^3, Z = 4, Mr = 297.30, Dc = 1.382 g/cm^3, F（000） = 616,/J = 0.090 mm^-1, S = 1.011, the final R = 0.0542 and wR = 0.1204 for 1669 observed reflections with I 〉 2σ（I） and 212 variable parameters. Hydrogen-bounding and n-stacking interactions were discussed. The influence of acetylene group on the fluorescence properties was also investigated. In comparison with N-phenyl-1,8-naphthalimide I （C18H11NO2）, few new structure characters and fluorescence properties of the title compound have been found.     

N,N'-亚水杨基皮考林酰肼合铜的晶体结构及荧光性质

N;N'-亚水杨基皮考林酰肼合铜的晶体结构及荧光性质     

Synthesis and Crystal Structure of a Novel Zincophosphite Containing Two-dimensional Inorganic-organic Network

IntroductionLowdimensionalcompoundsgenerallyincludeone-dimensionalchain-likeandtwo-dimensionallayer-likestructures.Theyhavereceivedconsiderableattentioninrecentyearsduetotheirstructuraldiversity,interestingunusualpropertiesdifferentfromthoseofthree-dimen-sionalcompounds,possibilitytotransformtohighdi-mensionalphase,andapplicationasspecialmaterials.1-3Inthelasttwoyearsseverallowdimensionalorgani-cally-templatedphosphiteshavebeenreported.4-6[HPO3]2-canmakethreelinkstoadjacentatomsviaP-O-M(M=Z…     

一个含苯甲酸配体的Mn-Ce混合金属簇合物的合成、晶体结构与磁性研究

本文使用(NH₄)₂Ce(NO₃)₆氧化Mn2+法合成了1个结构新颖的Mn-Ce混合金属簇合物[Mn₃Ce₂(O)₅(O₂CPh)₉(CH₃OH)₃]·2CH₃CN(1·2CH₃CN, HO₂CPh代表苯甲酸), 并对其进行元素分析、红外光谱、单晶X-射线结构分析、磁性等表征。结构分析表明, 化合物1·2CH₃CN属于三斜晶系P1空间群, 结构中2个Mn⁴⁺离子、2个Ce⁴⁺离子和4个桥连μ₃-O原子组成1个不规则的立方烷, 然后通过另1个桥连μ₃-O原子与另1个Mn³⁺离子相连。晶胞内分子间没有氢键作用, 但存在较强的π-π堆积作用。磁性研究表明, 簇合物内Mn离子之间存在铁磁性耦合作用, 基态自旋值S=5和磁各向异性参数D=-0.31 cm^-1, 交流磁化率没有频率依赖现象。     

一个含苯甲酸配体的Mn-Ce混合金属簇合物的合成、晶体结构与磁性研究

本文使用(NH4)2Ce(NO3)6氧化Mn2+法合成了1个结构新颖的Mn-Ce混合金属簇合物[Mn3Ce2(O)5(O2CPh)9(CH3OH)3]·2CH3CN(1.2CH3CN,HO2CPh代表苯甲酸),并对其进行元素分析、红外光谱、单晶X-射线结构分析、磁性等表征。结构分析表明,化合物1.2CH3CN属于三斜晶系P1空间群,结构中2个Mn4+离子、2个Ce4+离子和4个桥连μ3-O原子组成1个不规则的立方烷,然后通过另1个桥连μ3-O原子与另1个Mn3+离子相连。晶胞内分子间没有氢键作用,但存在较强的π-π堆积作用。磁性研究表明,簇合物内Mn离子之间存在铁磁性耦合作用,基态自旋值S=5和磁各向异性参数D=-0.31 cm-1,交流磁化率没有频率依赖现象。     

对氯苄基三苯基(鏻)-马来二氰基二硫烯镍配合物的合成和晶体结构

合成了一种新的含取代苄基三苯基鏻的马来二氰基二硫烯镍配合物[ClBzTPP]2[Ni(mnt)2].H2O([ClBzTPP]+代表对氯苄基三苯基鏻阳离子,mnt2-代表马来二氰基二硫烯阴离子).配合物为三斜晶系,空间群P墿,晶胞参数为a=1.058 5(2)nm,b=1.108 9(2)nm,c=1.157 0 nm,α=81.98(1)°,β=84.95(1)°,γ=84.45(1)°,V=1.369 1(4)nm3,Z=1,最终一致性因子R=0.058 4.该配合物由2个[ClBzT-PP]+阳离子,1个[Ni(mnt)2]2-阴离子和1个H2O组成.其结构特点是配合物中的[ClBzTPP]+阳离子和Ni(mnt)22-阴离子沿c轴方向堆积成柱,并通过C—H…S,C—H…π,C—H…Ni氢键和π-π堆积作用形成了二维网状结构.     

对氯苄基三苯基镌-马来二氰基二硫烯镍配合物的合成和晶体结构

合成了一种新的含取代苄基三苯基镌的马来二氰基二硫烯镍配合物[ClBzTPP]2[M（mnt）2]·H2O（[ClBzTPP]’代表对氯苄基三苯基锑阳离子,mnt^2-代表马来二氰基二硫烯阴离子）．配合物为三斜晶系,空间群Pi,晶胞参数为a=1．0585（2）nm,b=1．1089（2）nm,c=1．1570nm,α=81．98（1）°,β=84．95（1）°,γ=84．45（1）°,V=1．3691（4）nm^3,Z=1,最终一致性因子R=0．0584．该配合物由2个[ClBzT—PP]^＋阳离子,1个[M（mnt）2]^2-阴离子和1个H2O组成．其结构特点是配合物中的[C1BzTPP]’阳离子和Ni（mnt）2^2-阴离子沿c轴方向堆积成柱,并通过C—H…S,C—H…π,C—H…Ni氢键和π-π堆积作用形成了二维网状结构．     

含二芳胺基的吡啶甲酰胺的合成、晶体结构与除草活性

新化合物N-[2-(苯胺基)苯基]-2甲氧基吡啶-3-甲酰胺(C19H17N3O2)通过三步反应合成, 其结构通过1H-NMR, 13C-NMR, ESI-MS表征,其晶体结构通过 X-ray单晶射线衍射仪解析。该晶体属单斜晶系,空间群为P 1 21/n 1,晶胞参数为：a = 10.6329(18)?,b = 13.026(2) ?,c = 12.267(2) ?;Z =4, V =1669.7(5) ?3, Mr = 319.35, Dc = 1.270 mg/m3, S = 1.027, F(000) = 672, μ (MoKα) = 0.085 mm-1 ,可观测点精修最终偏离因子R = 0.0535 以及wR = 0.1353 和3854 个可观测点 I > 2σ(I). 晶体结构表明分子间存在氢键N(3)–H(3)???O(2)对晶体结构起到稳定的作用。初步除草活性表明,化合物N-[2-(苯胺基)苯基]-2甲氧基吡啶-3-甲酰胺在3000 g a.i/hm2对稗草的茎叶处理抑制率为91.81%。     

Synthesis and Crystal Structure of a Novel Hetero-six-nuclear Copper-iron Cluster Containing Ferroceylphenyl Groups

Ferrocene and the derivatives play an important role in organometallic chemistry due to their potential novel functions and applications. Of particular interest is an electron-transfer system of ion center for molecular electronics1. Several efforts have been directed towards the design and synthesis of multi-electron redox mediators that could transfer several electrons simultaneously at the same potential2. It was reported that ferrocenylphenyl group was an excellent electron transfer mediat…     

新颖的镧-2-氟苯甲酸及2，2′-联吡啶配合物的合成与晶体结构

2-fluorobenzoic acid (2-HFBA) and 2,2′-bipyridine (2,2′-bpy) was used as ligands to react with lanthanum to obtain a complex, [La(2-FBA)₃·(2,2′-bpy)]₂. The structure of the complex contains three independent molecules. In two of them, the two central metal ions are connected together through four 2-FBA groups by bidentate bridging and chelating-bridging two modes. In another, the two central metal ions are connected together through four bidentate bridging 2-FBA groups. CCDC: 237658.     

Synthesis,Crystal Structure and Photophysical properties of a Novel Molecule Containing a Triarylamine and an Oxadiazole Units

2-{3-[2-（4-N,N-Di-p-tolylaminophenyl)ethenyl]phenyl}-5-(4-bromophenyl)-1,3,4-oxadiazole(1) containing triarylamine and 2,5-diaryl-1,3,4-oxadiazole units was prepared by hornerWitting reactions.The structure of the compound was confirmed by ^1H NMR,IR ,MS and elemental analyses.The crystal structure of 1 was determined by X-ray diffraction analysis.UV absorpiton spectra and photoluminescent spectra were measured.     

Synthesis, Crystal Structure, and Herbicidal Activities of 2-Cyanoacrylates Containing 1,3,4-Thiadiazole Moieties

Three series of novel 2‐cyanoacrylates 7a – 7f , 9a – 9f , 10a – 10f containing 1,3,4‐thiadiazole ring moieties were synthesized as herbicidal inhibitors of photosystem II (PS II) electron transportation. Their structures were clearly verified by ¹H NMR, ¹³C NMR, elemental analysis (or HRMS analysis) and single‐crystal X‐ray diffraction analysis. Bioassay showed that a suitable group at the 3‐position of acrylates was essential for high herbicidal activity. In particular, compound 7e showed the best herbicidal activities and gave 100% inhibitory activity against rape and amaranth pigweed at a dose of 1.5 kg/ha. Introduction of substituent with higher polarity such as sulfinyl or sulfonyl to the 5‐position of 1,3,4‐thiadiazole decreased herbicidal activities.     

新型含吡啶环席夫碱的合成及其晶体结构

[N,N'-(2-胺基苯基)-2,6-二甲酰亚胺]吡啶分别与苯甲酰丙酮和4-甲氧基水杨醛通过缩合反应合成了新型含吡啶环席夫碱(1a和1b),其结构经X-射线单晶衍射,1H NMR,IR和元素分析表征.1a属三斜晶系,空间群P-1,晶体参数a=11.895(4)(A),b=12.584(4)(A),c=13.191(4)...