Novel hydrogen-bonded three-dimensional network complexes containing copper-pyridine-2,6-dicarboxylic acid

The novel complex (H₃O)₂[Cu(2,6-pydc)₂]·H₂O (pydc?=?pyridinedicarboxylic acid) (1) has been synthesized in aqueous solution and characterized by single-crystal X-ray diffraction, elemental analyses and IR spectra. X-ray structural analysis revealed that the novel complex possesses both π–π stacking and hydrogen-bonding interactions for three-dimensional (3D) networks. Crystal data for 1: a?=?13.454(3), b?=?10.266(2), c?= 13.783(3)?Å, α?=?90.00, β?=?115.29(3), γ?=?90.00°, Z?=?3, R ₁?=?0.0423, wR ₂?=?0.1217.     

Synthesis of novel copper compounds containing isonicotinic acid and/or 2,6-pyridinedicarboxylic acid: third-order nonlinear optical properties

Two novel compounds, [Cu₂(pydc)₂(inta)₂(H₂O)₂]·3H₂O 1 (pydc?=?2,6-pyridinedicarboxylic acid, inta?= isonicotinic acid) and [Cu(pydc)₂][Cu(H₂O)₅]·2H₂O 2, have been synthesized in aqueous solution and characterized by single-crystal X-ray diffraction, elemental analyses and IR spectra. Compound 1 exhibits reverse saturable absorption and self-defocusing. X-ray structural analysis reveals that Compounds 1 and 2 both possess π–π stacking and hydrogen-bonding interactions forming three-dimensional (3D) networks. Crystal data for 1: a?=?7.2345(14), b?=?12.219(2), c?=?17.069(3)?Å, α?=?90.44(3), β?=?91.82(3), γ?=?93.56(3)°, Z?=?1, R1?=?0.0435, wR2?=?0.1216. Crystal data for 2: a?=?8.3708(17), b?=?27.386(6), c?=?9.6170(19)?Å, α?=?90.00, β?=?98.14(3), γ?=?90.00°, Z?=?3, R1?=?0.0742, wR2?=?0.2160.     

Novel Hydrogen-bonded Three-dimensional Supramolecular Architectures Containing 2D Honeycomb Networks or 2D Grids

Two new supramolecular complexes,[Cu(H_2dhbd)(3-pyOH)(H_2O)]_2·3-pyOH·2H_2O(1)and[Cu_2(dhbd)(dpa)_2-(H_2O)]·6H_2O(2)(H_4dhbd=2,3-dihydroxybutanedioic acid,3-pyOH=3-hydroxypyddine,dpa=2,2'-dipyridylamine),have been synthesized in aqueous solution and characterized by single-crystal X-ray diffraction,elemental analyses,UV-Vis and IR spectra,and TGA analysis.X-ray structural analysis revealed that,through four pairs of strong O…H—O hydrogen bonds,the cyclic dinuclear units in 1 together with four adjacent neighbors are connected into a 2Dhoneycomb network encapsulating free 3-pyOH ligands.Unexpectedly,the water-dimers are fixed in interlayers of2D honeycomb network and act as hydrogen-bond bridging to further extend these 2D networks into 3D hydro-gen-bonded framework.Complex 2 includes interesting 2D grids constructed from chiral dinuclear units throughstrong O…H—O and O…H—N hydrogen bonding,which are extended through other crystallization water mole-cules into three dimension with channels.Variable-temperature magnetic susceptibility measurements for bothcomplexes indicate the presence of weak antiferromagnetic exchange interactions between adjacent copper(Ⅱ)ions.     

新型单核镍含氮配体配合物的合成及其性能

以苯胺-2,5-二磺酸钠（Na₂L）为原料,在水中,采用回流法合成了一种Ni²⁺有机配合物［Ni(phen)₂(H₂O)₂］(L)·3H₂O（1,phen=1,10-邻菲啰啉）,其结构经IR, 元素分析, X-射线单晶衍射和TGA表征。结果表明：1属三斜晶系,P1空间群,晶胞参数a=9.926 0(8) ,b=11.467 9(9) , c=14.486 1(12) , V=1 608.7(2) ³, Z=2, Dc=1.570 g·cm^-3。研究了1的荧光性质,热稳定性和磁学性质。结果表明： 1的荧光发射峰与配体相比发生明显红移,具有较高的热稳定性和铁磁耦合作用。     

A Novel Humidity-Sensitive Material Based on PDEB with Nickel Complex Catalyst

lntr0ducti0nHumidityisaveryimportantphysicalpr0perty,andinrecentyears,theresearch0nhu-miditysensors,whichfocused0nl0okingforproperhumidity-sensitivematerials,hasattractedmoreandmoreattentionw0rldwide.l~2PDEBisahydrophobicpoIymerwithhighrr-c0njugatedstructure,whichpresentsitwithpotentialapplicationinelectr0nics.'~'Inourrecentstudy,itwasfoundtobesensi-tivetohumiditychange,whichmakesitap0tentialhumidity-sensitivematerialf0rhu-miditysensors.However,acc0rdingt0literatures,PDEBpreparedisinsoluble…     

一种新型羟基铅配合物的合成及其荧光性质

以3,5-吡唑二甲酸(H₃pdc)为配体,Pb(NO₃)₂为金属盐,在水热反应条件下通过调节pH,合成了一种新的二维羟基Pb配合物--［Pb₂OH(pdc)(H₂O)·H₂O］_n(1),其结构经IR,元素分析和X-射线衍射表征。1(CCDC: 1 469 184)属单斜晶系,P2₁/n空间群,晶胞参数a=10.502(2) , b=9.176 5(2) , c=10.602(2) , β=97.417(7)°, V=1 013.2(3) ³, Z=4, R₁=0.022 4, wR₂=0.045 8, S=1.02。每个不对称结构单元中具有两种不同配位环境的Pb,在同一结构单元中,2个Pb通过羟基O相连,相邻不对称结构单元通过配体连接Pb(Ⅱ)形成二维网络结构。荧光发射光谱研究结果表明：在最大激发波长(264 nm)激发下,1在380 nm, 419 nm和440 nm附近显示出较强的荧光性能。     

新型镍配合物的溶剂热合成及其晶体结构

以2-乙氧基-6-亚氨甲基苯酚(HL)为配体,与氨水和Ni(ClO4)2.6H2O经溶剂热法合成了新型镍配合物[Ni(L)2](1),其结构经IR,元素分析和XRD表征。1属三斜晶系,Pī空间群,晶胞参数a=0.843 3(3)nm,b=1.009 4(2)nm,c=1.188 4(2)nm,α=111.16(3)°,β=97.43(3)°,γ=102.43(3)°,V=0.897 2(11)nm3,Mr=387.05,Z=2,Dc=1 433 g.cm-3,F(000)=404,μ=1.105 mm-1,S=1.015。1中Ni2-分别与两个L-上的两个N原子和两个O原子配位,形成了平面四边形几何构型。分子通过一对N-H┈O氢键形成二聚体;二聚体进一步通过N-H┈O氢键和C-H┈Ni氢键的相互作用形成二维网状结构。     

Synthesis of a Novel Ligand Containing Phenyl Pyridine

In this article, we provide a new, efficient route to synthesize 2-[3-(3,4-bis(2-ethylhexyloxy)phenyl]phenyl pyridine ligand from readily available starting materials. The target compound was obtained by a condensation reaction and Suzuki coupling reaction. Structures of compounds were demonstrated by ¹H NMR, ¹³C NMR, and high-resolution mass spectrometry. The advantages of this synthetic route are simple operation, mild reaction conditions, and good yields.     

一种新型含磷-溴-氮阻燃剂的合成

以三氯氧磷、季戊四醇、2 ,3-二溴丙醇及三聚氰胺等为原料合成了一种新型磷 -溴 -氮阻燃剂 0 - (2 ,4,6 -三氧杂 - 1-氧基磷杂双环 [2 .2 .2 ]辛烷 - 4-亚甲基 ) - 0 - 2 ,3- (二溴丙基 )磷酸三聚氰胺盐 (Ⅲ ) .改进了中间体 4-羟甲基 - 2 ,6 ,7-三氧杂 - 1-氧基磷杂双环 [2 .2 .2 ]辛烷 (Ⅰ )的合成条件 ,元素分析、红外光谱等确定了结构     

Hydrogen-bonded assemblies of trinuclear metal string complexes

Three kinds of trinuclear metal string complexes, [Ni₃(dpa)₄(L¹)₂]?·?H₂O?·?C₂H₅OH (L¹?=?(E)-3-(2-hydroxyl-phenyl)-acrylic acid) (1), [Ni₃(dpa)₄(L²)₂]?·?2C₂H₅OC₂H₅ (L²?=?(E)-3-(3-hydroxyl-phenyl)-acrylic acid) (2) and [Ni₃(dpa)₄(L³)₂]?·?3CH₂Cl₂?·?1.5CH₃OH (L³?=?(E)-3-(4-hydroxyl-phenyl)-acrylic acid) (3). (dpa^??=?bis(2-pyridyl)amido), have been synthesized. The structures of 1 and 2 have been analyzed by the X-ray single-crystal diffraction showing hydrogen-bonded networks.     

非达司他的合成新方法

发展一条醛糖还原酶抑制剂非达司他的新合成方法,以价廉、易得的N-苯基马来酰亚胺和对氟苯酚为原料,在碱催化下经Oxo-Michael加成反应、水解、(S)-α-苯乙胺拆分、Friedel-Crafts酰化反应得(S)-6-氟-3,4-二氢-4-氧-2H-1-苯并吡喃-2-羧酸,进一步经Bucherer-Bergs乙内酰脲化反应和氯化4-(4,6-二甲氧基-1,3,5-三嗪-2-基)-4-甲基吗啉盐(DMT-MM)作用下的酰胺化反应得目标物,7步反应总收率22.4%.所有中间体和目标物经1H NMR,13C NMR,HRMS及比旋光度确证并与文献值比较.该方法原料易得、反应条件温和,操作简便,收率良好,产物分离纯化容易,适合大规模制备非达司他.     

配合物Ru(dcbpy)(phen)2(PF6)2的2D-NMR分析

用一维ＮＭＲ方法研究了新型电化学发光探针Ｒｕ（ｄｃｂｐｙ）（ｐｈｅｎ）２（ＰＦ６）２的立体结构,借助二维＾１Ｈ－＾１Ｈ ＣＯＳＹ和＾１Ｈ－＾１３Ｃ ＣＯＳＹ实验对其氢谱和碳谱进行了完全的归属,并给出了其氢谱和碳谱的化学位移值。     

Synthesis and Crystal Structure of a New Nickel(II) Complex with Unsymmetric Quadridentate Schiff Base Containing Oxime

1 INTRODUCTION The interest in the complexes of transition met-als with ketoxime ligands[1, 2] as potential modelsfor metal binding sites in ferroverdin[3, 4] hasprompted the investigations on the structures andthe overall coordination geometry of the metalcenters in these complexes. Oxime derivatives areinteresting ligands since the ketoximes are foundto chelate transition metals through the N (oxime)and O (ketone) donors[5～10]. Herein we report thesynthesis…     

Hetero-bimetallic Complex of a 2D Coordination Network Constructed by Sodium Ion and p-Sulfonatothiacalix[4]arene

A 2D coordination polymer built by sodium ion and water-soluble p-sulfonatothiacalix[4]arene of trivalent yttrium complex [Na（H2O）2Y（H2O）6（DMF） （p-sulfonatothiaca lix[4]arene）]-9H2O is reported. The complex belongs to the monoclinic system, space group P2 1/c, with a = 16.703（3）, b = 17.819（4）, c = 17.357（4）A, β = 106.23（3）°, Z = 4, V = 4960.0（17）A^3, Mr = 1304.08, Dc = 1.746 g/cm^3,μ= 1.624 mm^-1, F（000） = 2688, the final R = 0.0398 and wR = 0.1132 for 7534 observed reflections with I 〉 2σ（I）. One yttrium（Ⅲ） ion is coordinated by the thiacalixarene ligand via the sulfonato group, and also ligated by an oxygen atom of a DMF molecule occupying the cavity of thiacalixarene and six aqua ligands.     

Synthesis and Crystal Structure of Zinc(II) Complex with Isonicotinate Containing a Three-dimensional Hydrogen-bond Network

1 INTRODUCTION Because isonicotinic and nicotinic acids play an important role in the metabolism of all living cells and their metal complexes can also be used as a drug[1]. Much interest has been directed towards the synthesis and structure investigation of these metal complexes[2,3]. With the zinc(II) complex, a trans-octahedral structure [Zn(NIC)2(H_2O)4] (NIC= C6H4NO2), has been ascertained by X-ray analysis[4]. Herein we report the synthesis and crystal structure of the title c…     

Synthesis of Heterocycle Compounds Containing Two Pyridazinone Units

Four novel compounds containing two pyridazinone units attached to one benzene or pyridine ring, protected and deprotected 1,5-di[3（2H）-pyridazinon-6-yl]benzene and 2,6-di[3（2H）-pyridazinon-6-yl]pyridine were synthesized in eight steps, which provided a useful method for the preparation of pyridazinone derivatives via the Stetter and cyclization reactions. Their structures were characterized by ^1H NMR, ^13C NMR, and HRMS.     

一种新三维描述子用于Nevirapine类抗艾滋病药物定量构效关系的研究

运用三维全息原子场作用矢量(3D-HoVAIF)对33个Nevirapine类抗艾滋病药物进行了定量构效关系(QSAR)研究。采用偏最小二乘回归(PLSR)建立定量构效关系模型,同时采用内部及外部双重验证的方法对所得模型稳定性能进行深入分析和检验,所建模型的复相关系数(Rcum2)、留一法(LOO)交互校验(CV)复相关系数(Qcum2)和外部样本校验复相关系数(Qext2)分别为0·835、0·530和0·518。结果表明,3D-HoVAIF能较好表征Nevirapine类抗艾滋病药物分子结构信息,且所建模型具有较好稳定性能和预测能力。     

Ni2L配合物的热稳定性和电化学研究

用金属离子作模板通过N－氧化吡啶－2，6－二甲醛与1，3－丙二胺缩合得到了新型大环水溶性希夫碱金属配合物Ni2LCl6·C2H5OH·10H2O，对其进行了元素分析、红外光谱、电化学及热稳定性能的研究．结果显示：Ni2L配合物的电极反应可以认为是一个双电子传输过程，并且电极过程是一个不可逆过程，求得它的扩散系数为4．07×10－6cm2·s-1．该配合物的稳定性较好，约在563℃配合物发生分解，失去有机基因，生成氧化物．     

Synthesis and Crystal Structure of a Distorted 2D （6,3） Layer Complex, [Cd（H2mbdpz）（N3）2]n （H2mbdpz = 4,4′-Methylenebis（3,5-dimethylpyrazole）） Containing both End-on and End-to-end Azide Bridges

The complex [Cd（H2mbdpz）（N3）2]n 1 （H2mbdpz = 4,4′-methylenebis（3,5-dimethylpyrazole）） has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in the monoclinic system, space groups C2/c with a = 22.154（5）, b = 7.4835（15）, c = 21.044（8）A^°,β= 115.51（3）°, V= 3148.7（17）A^°3, Z= 8, C11H16CdN10, Mr = 400.75, Dc = 1.691 g/cm^3,μ = 1.401 mm^-1, F（000） = 1599, T= 293（2） K, the final R = 0.0228 and wR = 0.0581 for 3604 observed reflections with I 〉 2σ（I）. The structural determination revealed that the coordination environment of Cd（Ⅱ） atom is a distorted octahedron consisting of two nitrogen donors of two H2mbdpz ligands and four nitrogen donors from four azide ligands. The azide moieties act as bridges in two modes： end-on （μ1,1-） and end-to-end （μ1,3-）, and H2mbdpz also serves as a bridge with a bis-monodentate coordination. Both bridging ligands link the Cd（Ⅱ） atoms to form a distorted two-dimensional （6,3） layer.     

Synthesis of monodisperse poly(methacrylic acid) microspheres by distillation-precipitation polymerization

Monodisperse poly(methacrylic acid) (PMAA) microspheres were prepared by distillation-precipitation polymerization in acetonitrile with 2,2′-azobisisobutyronitrile (AIBN) as initiator. The polymeric microspheres were formed simultaneously via a precipitation polymerization manner during the distillation of the solvent out of the reaction system in the absence of any surfactant and crosslinker. Monodisperse PMAA microspheres with spherical shape and smooth surface were synthesized with diameters ranging from 60 to 290 nm below the glass transition temperature of PMAA without any stabilizer. The particle size increased with increasing monomer concentration, which may be resulted from the higher molecular weight for the polymerization. To investigate the growth procedure of PMAA microspheres, the morphology of microspheres over the distillated acetonitrile volume was conducted by monitoring the morphologies with TEM. GPC and FTIR provide key insights into the particle growth mechanism. The PMAA microspheres may be formed by an internal contraction due to the marginal solvency of the continuous phase with the aid of the hydrogen-bonding interaction between the carboxylic acid unit, in which the particles were stabilized by the steric effect of the pendent chains and surface gel as well as the electrostatic repulsion from the carboxylic acid group.