Synthesis and Crystal Structure of 1,4-Bis(2-hydroxymethylphenyl)-1,4-dioxabutane

1 INTRODUCTION Macrocyclic ligands and their metal complexes have received much attention due to their applications in ion transport, ion separation and as models in biomimic researches[1~7]. The synthetic methods of macrocyclic ligands and their metal complexes are mainly divided into three kinds[8]. The first one is synthesizing free ligand, then forming the metal complexes; the second is template synthesis; and the third is synthesizing the end-off or side-off precursor ligand, then c…     

Synthesis and Characterization of 2,6-Bis(imino)phenoxy Cobalt Complexes

ＩｎｔｒｏｄｕｃｔｉｏｎＲｅｃｅｎｔｒｅｓｅａｒｃｈｅｆｆｏｒｔｓｈａｖｅｂｅｅｎｄｅｖｏｔｅｄｔｏｔｈｅｓｔｕｄｙｏｆｌａｔｅｔｒａｎｓｉｔｉｏｎｍｅｔａｌｃｏｍｐｌｅｘｅｓａｓｍｏｄｅｌｓｙｓｔｅｍｓｆｏｒｔｈｅｐｏｌｙｍｅｒｉｚａｔｉｏｎｏｒｏｌｉｇｏｍｅｒｉｚａｔｉｏｎｏｆｅｔｈｙｌｅｎｅ .1 3ＴｈｅｍｏｓｔｎｏｔａｂｌｅａｃｈｉｅｖｅｍｅｎｔｓｈａｖｅｂｅｅｎｄｏｎｅｂｙＢｒｏｏｋｈａｒｔ,4 Ｂｅｎｎｅｔｔ,5ａｎｄＧｉｂｓｏｎｇｒｏｕｐｓ .6,7Ｔｈｅｙｉｎｄｅ ｐｅｎｄｅｎｔｌｙｒｅｐｏｒ…     

New Coordination Polymers of 1,4-Bis(2″-Hydroxyphenylazomethine) Phenylene

Coordination polymers of 1,4-bis(2′-hydroxyphenylazomethine) phenylene have been prepared with the metal ions Ti(III), Cr(III), Fe(III), Mn(II), Ni(II), and Cu(II). They were characterized by elemental analysis, IR, and electronic spectra. The metal contents in all polymers were found to be consistent with a 1:1 (metal:ligand) stoichiometry. The thermal behavior of these coordination polymers has been studied by thermogravimetric analysis in air up to 750°C, and the data showed that they are thermally stable up to 200°C. Physical properties such as the solubility and viscosity of the polymer complexes were also determined. Electrical conductivity measurements of the synthesized polychelated polymers showed that they are insulators except for the Ni(II) complex which shows a semiconducting character. Mössbauer data clearly establish the 3 + oxidation state for the iron complex polymer.     

Syntheses,Crystal Structures,and Photoluminescent Properties for One New Cd(Ⅱ) CP Based on 3,5-Bis(4?-carboxy-phenyl)-1,2,4-triazole and 1,4-Bis(imidazol-1-ylmethyl)benzene

One new coordination polymer(CP) [Cd(bct)(bib)]·2(H_2O)(1), based on 3,5-bis(4?-carboxy-phenyl)-1,2,4-triazole(H2 bct) and 1,4-bis(imidazol-1-ylmethyl)benzene(bib), has been synthesized by hydrothermal method, and its structure was determined and characterized by single-crystal X-ray diffraction analysis, elemental analysis, IR spectroscopy, and thermogravimetric analysis. The crystal structure of CP 1 is a three-dimensional framework with(3,5)-connected topology, where the bct ligands adopt a μ3-kO,kO,kO coordination mode connecting with three Cd centers and the bib ligands adopt a μ2-k N,k N coordination mode bridging two Cd ions. It crystallizes in monoclinic system, space group C2/c, with a = 2.6838(4), b = 1.24221(17), c = 1.8011(2) nm, β = 102.939(2)o, V = 5.8522(13) nm3, Z = 8, C30 H27 CdN7O6, Mr = 694.00, Dc = 1.566 g/cm~3, F(000) = 2784, S = 1.055, R = 0.0294 and wR = 0.0731. Furthermore, solid-state photoluminescence measurements show that CP 1 produces strong emissions at room temperature.     

Synthesis,Crystal Structure and Properties of a New Cadmium Compound with(1,1?-(1,4-Butanediyl)bis(imidazole) and p-Hydroxybenzoic Acid

A new metal-organic framework based on bbi and PHBA(bbi = 1,1?-(1, 4-butanediyl)bis(imidazole), PHBA = p-hydroxybenzoic acid), namely, [Cd(bbi)(PHBA)_2]_n(1) has been synthesized by the conventional method. Compound 1 displays a two-dimensional(2D) layer structure possessing the left-and right-handed helical chains and stabilized by intermolecular hydrogen-bonding to form a three-dimensional(3D) supramolecular structure. Topologically, the 2D layer belongs to well-known(4,4) network topology. The structure has been determined by single-crystal X-ray diffraction analyses, and further characterized by infrared spectra(IR), elemental analyses and powder X-ray diffraction. In addition, the thermal behavior and luminescent properties of [Cd(bbi)(PHBA)_2]_n have been investigated in detail.     

Synthesis of N,N′-Bis(arylsulfanyl)cyclohexa-2,5-diene-1,4-diimines and N,N′-(Cyclohexa-2,5-diene-1,4-diylidene)bis(arenesulfinamides)

Russian Journal of Organic Chemistry - Reactions of (chlorosulfanyl)benzenes with benzene-1,4-diamines afforded new N,N′-bis(arylsul­fanyl)cyclohexa-2,5-diene-1,4-diimines which were...     

A Novel Method for Synthesizing 4,4′-Bis(hydroxymethyl)-2,2′-bipyridine

IntroductionSince C. W. Tang firstly reported theelectroluminescence of 8- hydroxyquinolinealuminium[1] ,much attention has been paid to themetal complexes as electro- luminescent materials.Based on a series of experimental data,it has beenknown that the electroluminescence of metalcomplexes with heterocyclic ligands containing Nand O elements mainly results from the tripletstatetransition.For some transitional metal complexes,there exist the transitions from metal to ligand( MLCT) at thei…     

A One-dimensional Cd(Ⅱ) Coordination Polymer Constructed from 1,4-Benzene-dicarboxylic Acid and 3-(2,6-Di(pyrazin-2-yl)pyridin-4-yl)-1H-indole:Synthesis,Structure and Photoluminescence

A new coordination polymer {[Cd(C_(21)H_(14)N_6)(C_8H_4O_4)]·H_2O}_n(1) was synthesized by an elaborate design via the reaction of 3-(2,6-di(pyrazin-2-yl)pyridin-4-yl)-1H-indole(bppi),1,4-benzene-dicarboxylic acid(H2bdc) and cadmium(Ⅱ) nitrate in CH_3OH/H_2O mixed solvents. Complex 1 crystallizes in orthorhombic,space group Ccca with a = 20.012(4),b = 31.881(6),c = 19.808(4) ?,V = 12638(4) ?~3,Z = 16,C_(29)H_(20)CdN_6O_5,M_r = 644.91,D_c = 1.356 g·cm~(-3),μ = 0.735 mm~(-1),F(000) = 5184,GOOF = 1.046,the final R = 0.0405 and wR = 0.1063 for 6870 observed reflections(I 2σ(I)). The Cd(Ⅱ) centre is hepta-coordinated by three N and four O atoms from one bppi terminal ligand and two bdc2– ligands,respectively,displaying a capped trigonal prism geometry. Structure extension gives coordination polymeric chains,in which the bdc2– linkers connect Cd(Ⅱ) cations into a one-dimensional(1D) coordination polymer along the c axis,giving zigzag chains with the Cd···Cd separation of 11.178(1) ?. The adjacent bppi terminal ligands in the chains are anti-periplanar conformation. The three-dimensional(3D) structure is stabilized by π···π stacking and hydrogen-bonding interactions to form a supramolecular self-penetrating network with 1D channels. In 1,there are voids 2999.7 ?~3 with 23.7% of per unit cell volume. Thermal analysis indicates that the framework of 1 is stable until 651 K and the photoluminescence of 1 in the solid shows very weak fluorescence at 382 and 560 nm upon excitation at 310 nm.     

A new Compound from Chaenomeles sinensis (Thouin) Koehne

A new dihydrochromone derivative,named chaenomone,was isolated from the twigs of Chaenomeles sinensis (Thouin)Koehne .The structure was determined by spectroscopic methods.     

A New 2D Zinc(Ⅱ)Coordination Polymer Constructed by Imidazole-4,5-dicarboxylic Acid(H3IDC)and 1,4-Bis(imidazol-l-ylmethyl)-benzene(bix)

T A new 2D Zn(Ⅱ)coordination polymer[Zn(HIDC)(bix)0.5]n(1)was obtained by the hydrothermal reaction of ZnCI2,imidazole-4,5-dicarboxylic acid(H3IDC)and 1,4-bis(imidazol-1-ylmethyl)-benzene(bix)with a 2:2:1 mole ratio.X-ray diffraction crystal structural analysis reveals it crystallizes in monoclinic,space group P21/n with α=12.125(3),b=10.541(3),c=684,μ(MoKα)=1.730 mm-1,the final R=0.0439 and wR=0.0888 for 2101 observed reflections with Ⅰ＞2σ(Ⅰ).In 1,each zinc(Ⅱ)ion is five-coordinated with a slightly distorted trigonal bipyramidal coordination geometry,and each μ2-HIDC2-acts as a bridge to bond two neighboring Zn(Ⅱ)ions,leading to a 1D zigzag chain architecture.The adjacent zigzag chains are further linked by μ2-bix to form an infinite 2D network structure.The fluorescence spectrum of 1 exhibits intense emission at 466 nm when excited at 397 nm in solid state at room temperature.     

4-(3-羟基苯基)-2,6-二甲基-1,4-二氢吡啶-3,5-二羧酸乙酯的合成和晶体结构

标题化合物C19H23NO5由间羟基苯甲醛、碳酸氢铵、乙酰乙酸乙酯在乙醇溶剂中回流制备.结构通过单晶X-射线衍射法测定,其晶体属三斜晶系,空间群Pi,a=7.4550(15),b=8.9780(18),c=14.099(3)(A),α=80.22(3),β=86.72(3),γ=68.62(3)°, V=865.9(3)(A)3, Z=2, Mr=345.38, Dc=1.325g/cm3, F(000)=368. 晶体结构用直接法解出,经全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R1=0.0633,wR2=0.1709[I＞2σ(I)].在晶体结构中,二氢吡啶环与苯环之间的二面角为90.0(2)°,分子通过氢键形成有隧道的一维超分子结构.     

1,4-二氢-2,6-二甲基-4-(3-硝基苯基)-3,5-吡啶二羧酸二(2-甲氧基乙基)酯的合成

对1，4－二氢吡啶类钙拮抗剂西尼地平进行了结构修饰。以双乙烯酮和乙二醇单甲醚为原料，经酯化、缩合、氨化和Hantzsch环化等反应合成了1，4－二氢－2，6二甲基－4－（3－硝基苯基）－3，5－吡啶二羟酸二（2－甲氧基乙基）酯，总收率71％。目标产物结构经^1H NMR和MS确证。     

Bicyclic Phenyl–Ethynyl Architectures: Synthesis of a 1,4-Bis(phenylbuta-1,3-diyn-1-yl) Benzene Banister

The novel diacetylene bridged terphenylic macrocycle 1 is presented and discussed in the context of rotationally restricted “Geländer” oligomers. The 1,4-bis(phenylbuta-1,3-diyn-1-yl) benzene bridge of diacetylene 1 is significantly longer than its terphenyl backbone, forcing the bridge to bend around the central pylon. The synthesis of molecule 1 is based to a large extent on acetylene scaffolding strategies, profiting from orthogonal alkyne protection groups to close both macrocyclic subunits by oxidative acetylene coupling sequentially. The spatial arrangement and the dynamic enantiomerization process of the bicyclic target structure 1 are analyzed. In-depth NMR investigations not only reveal an unexpected spatial arrangement with both oligomer strands bent alongside the backbone, but also display the limited stability of the model compound in the presence of molecular oxygen.     

4,4′-(1,4-苯撑)-双-(N-甲基-2,6-二苯基)双吡啶盐与四苯基磺酸锌卟啉相互作用研究

在可见光照射下,水溶性的四苯基磺酸锌卟啉(ZnTPPS),当有还原剂存在时,可使连吡啶双盐如甲基紫精MV~(2+)还原成一价甲基紫精MV_·~+。在铂催化剂存在下,MV_·~+又可将H_2O还原成H_2。由于H_2是一个重要能源,此反应近年来深受重视。 4,4′-连吡啶双盐与ZnTPPS的相互作用已有报导,但中间夹一个苯基的双吡     

Synthesis,Crystal Structure,and Catalytic Performance of 2,6-Bis[1-(2,4,6-trimethylphenylimino)ethyl]pyridine Nickel(Ⅱ)Complex

A novel nickel(Ⅱ) complex Ni[L]Cl2·CH3CN(1) containing the tridentate ligand 2,6-bis[1-(2,4,6-trimethylphenylimino)ethyl]pyridine(L) has been synthesized. The crystal structure of complex 1 was determined by single crystal X-ray diffraction analysis. The catalytic activity of complex 1 for the polymerization of ethylene was studied under activation with methylaluminoxane(MAO).     

2,3; 6,7-Bis (2′,3′-quinolino)tcu: A rigid syn-orthocyclophane

A bis 2,3-quinoline fused derivative of tetracyclo[6.2.1.0.0]undecane is prepared by two sequential Friedlander condensations. An X-ray crystal structure indicates a dihedral angle of 50.5° between the two quinoline rings.     

A Convenient Synthesis of β,β-Bis(Alkylthio)Acrylonitriles

We describe a useful synthesis of a variety of β,β-bis(alkylthio)acrylonitriles via the alkylation of the salt arising from the condensation of acetonitrile with carbon disulfide in ether.     

A New 2D Zinc(Ⅱ) Coordination Polymer Constructed by Imidazole-4,5-dicarboxylic Acid(H_3IDC) and 1,4-Bis(imidazol-1-ylmethyl)-benzene(bix)

A new 2D Zn(Ⅱ) coordination polymer [Zn(HIDC)(bix)0.5]n(1) was obtained by the hydrothermal reaction of ZnCl2,imidazole-4,5-dicarboxylic acid(H3IDC) and 1,4-bis(imidazol-1-ylmethyl)-benzene(bix) with a 2:2:1 mole ratio.X-ray diffraction crystal structural analysis reveals it crystallizes in monoclinic,space group P21/n with a = 12.125(3),b = 10.541(3),c = 12.484(3) ,β = 115.834(4)°,V = 1436.0(6) 3,Mr = 338.60,Z = 4,Dc = 1.566 Mg·m-3,F(000) = 684,μ(MoKα) = 1.730 mm-1,the final R = 0.0439 and wR = 0.0888 for 2101 observed reflections with I ≥ 2σ(I).In 1,each zinc(Ⅱ) ion is five-coordinated with a slightly distorted trigonal bipy-ramidal coordination geometry,and each μ2-HIDC2-acts as a bridge to bond two neighboring Zn(Ⅱ) ions,leading to a 1D zigzag chain architecture.The adjacent zigzag chains are further linked by μ2-bix to form an infinite 2D network structure.The fluorescence spectrum of 1 exhibits intense emission at 466 nm when excited at 397 nm in solid state at room temperature.