一维梯子状配位聚合物[Na3Er(2，6-PDA)3]·11.5H2O的合成与晶体结构

A novel 1D Ladder-like coordination polymer [Na₃Er(2，6-PDA)₃]·11.5H₂O (2,6-H₂PDA is pyridine-2,6-dicarboxylic acid) has been synthesized and the crystal structure was determined by X-ray diffraction. The crystal structure of the complex belongs to Monoclinic system with space group P2₁/c, a=0.969 7(3) nm, b=1.914 6(6) nm, c=1.8031(6) nm, β=91.524(5)°, V=3.346 6(18) mm³, Z=4, D_c=1.863g·cm^-3, μ=2.645 mm^-1. The coordination geometry configuration of Er³⁺ center is tricapped trigonal prism. The structures of the title compound exhibit a novel 1D Ladder-like chain.     

The Friedel-Crafts Acylation of Substituted Benzene with 2 - Phenylfuran-3, 4-dicarboxylic Acid Anhydride

TheFriedel-Craftsacylationreactions'-2areofparticularvalueowingt0theselectivityandeasewithwhichtheyareusuallyacc0mPlished,thusprovidingusefulroutestohighlyfimctionalinedar0maticringsystems.Sincesesamin-grouPlignanshavetW0aro-maticmoieties,theaPplicationoftheFriedel-CraftsacylationreactioninourstratCgyforsynthesisofsuchlignansseemedprondsing.Hence,titlecomPoundlwaschosenastheacylatingagenttoexaminesuchfeasibility.Ourresearchw0rkwasstartedfrom2,4-diphenyloxazole2,theprepaxation0fwhichwasgrea…     

Synthesis and Crystal Structure of [Zn(HPDB)_2(H_2O)_2]n·2nDMSO·2nH_2O (H_2-PDB = Pyridine-3,4-dicarboxylic Acid)

1 INTRODUCTION Metal-organic coordination polymers are currently of considerable interest and importance because they can be used as new functional materials applicable in adsorption, luminescent and NLO materials fields[1, 2]. Due to the manifold N- and O-donors of pyridine- (bi)carboxylic ligands, metal pyridine-(bi)carboxyla- tes can construct versatile structural motifs, which finally aggregate to generate various supramolecular architectures with interesting properties[3, 4]. The d…     

Synthesis,Crystal Structure and Magnetic Behavior of a New Manganese（Ⅱ） Coordination Polymer [Mn（DPPZ）（PZDC）（H2O）] （DPPZ = Dipyrido[3,2-a：2＇,3＇-c] -phenazine and H2PZDC = Pyrazine-2,3-dicarboxylic Acid）

The title complex, [Mn（DPPZ）（PZDC）（H2O）] 1 （DPPZ = dipyrido[3,2 -a：2＇,3＇- c]phenazine and H2PZDC = pyrazine-2,3-dicarboxylic acid）, has been hydrothermally synthesized and structurally characterized by X-ray single-crystal diffraction, elemental analyses, IR, TG- DTA and magnetic susceptibility measurement. It crystallizes in triclinic, space group P1^- with a = 6.6842（5）, b = 7.5741（6）, c = 20.5755（15）A, α = 90.1160（10）, β = 97.0560（10）, γ = 97.3350（10）°, V= 1025.16（13）A^3, Z = 2, MnC24H14N6O5, Mr= 521.35, Dc= 1.689 g/cm^3, F（000） = 530, μ（MoKa） = 0.699 mm^-1, R = 0.0366 and wR = 0.0810. Compound 1 contains one- dimensional chains which are further stacked through π-π interactions to form a 3D supramolecular architecture. The water molecule O（1W） is involved in hydrogen bonding interactions with symmetric carboxylate oxygen atom 0（4） at （x＋ 1, y＋1, z） and symmetric PZDC nitrogen atom N（6） at （1-x, 1-y, 1-z）, which completes the structure of 1. Magnetic susceptibility measurement indicates that the compound behaves a weak antiferromagnetic exchange interaction.     

Synthesis and Crystal Structure of 3-(Pyrrole-2''-carboxamido)propanoic Acid·(1/2)H2O

3-(Pyrrole-2'-carboxamido)propanoic acid I has been synthesized from the reaction of β-alanine methyl ester with 2-trichloroacetylpyrrole followed by saponifying and acidating in 85.4% yield, and the crystal structure of 3-(pyrrole-2'-carboxamido)propanoic acid· (1/2)H2O (C8H11N2O3.5, Mr = 191.19) was obtained and determined by X-ray diffraction method. The crystal is of monoclinic, space group C2/c with a = 19.010(4), b = 8.3515(17), c = 13.788(3) (A), β = 125.88(3)°, V = 1773.6(6) (A)3, Z = 8, Dc = 1.432 g/cm3, λ = 0.71073 (A), μ-MoKα) = 0.114 mm-1 and F(000) = 768. The structure was refined to R = 0.0354 and wR = 0.0942 for 1642 observed reflections with I > 2σ(I). It is revealed that the title compound has one pyrrole ring and one propionic acid subchain linked by an amido bond at C(4), and there are 8 molecules of com- pound I and 4 crystal water molecules in each unit cell. The supramolecular layers are stabilized by the hydrogen bonds of N(2) H…O(2), N(1) H…O(4), O(4) H(1W)…O(2) and O(3) H…O(1).     

3-硝基-2-氨基苯甲酸的合成

以邻苯二甲酸酐为起始原料,经硝化、脱水、酰胺化、霍夫曼重排4步反应合成了3-硝基-2-氨基苯甲酸,总收率19%,其结构经1H NMR, IR和元素分析表征.探讨了酰胺化和霍夫曼重排反应条件对产率的影响.结果表明, n(脲素) ∶ n(3-硝基邻苯二甲酸酐)=2.0 ∶ 1.0,于50 ℃～60 ℃反应5 h～6 h,酰胺化反应收率85%～91%.n(NaClO) ∶ n(3-硝基-2-甲酰胺基苯甲酸)=1.2 ∶ 1.0,于60 ℃反应3 h,重排反应收率94%.     

含吡嗪甲酸配体的双核铬配合物的水热合成、晶体结构及荧光性质

通过水热法合成了1个双核铬配合物[Cr2(OH)2(2-pca)4].3H2O(2-Hpca=2-吡嗪甲酸),并对其进行了X-射线单晶衍射、红外光谱、元素分析、荧光和热的表征及研究。该配合物属于单斜晶系,P21/c空间群。晶体学数据:a=1.566 35(15),b=0.847 70(6),c=1.974 60(18)nm,β=90.645 0(10)°,C20H20Cr2N8O13,Mr=684.44,V=2.621 7(4)nm3,Dc=1.734 g.cm-3,F(000)=1 392,μ=0.913 cm-1,Z=4,最终R=0.044 7,wR=0.112 0用于3 251个可观测点。在晶体结构中,每个铬原子均为六配位,其中来自两分子2-吡嗪甲酸的2个氮原子、2个羧酸基氧原子和2个桥连羟基上的氧原子,呈现畸变的八面体几何构型。     

Synthesis and Crystal Structure of 3-(Pyrrole-2′-carboxamido)propanoic Acid·(1/2)H_2O

1 INTRODUCTION Pyrrole and its derivatives have attracted much attention due to their chemical properties as well as biological activities[1]. They have been widely used to produce pharmaceutical, essences, biochemicals, etc. It has been found that a great number of pyrrole derivatives present antitumor and antiviral activi- ties[2 ~ 5]. During our searches for bioactive com- pounds, a series of pyrrole derivatives were synthe- sized[6, 7]. We report here the synthesis of 3-(pyrrole- 2?-…     

异核配合物K2[Co(Dipc)2]·7H2O的合成、性质、结构和热分解动力学研究

A heteronuclear compound, K₂[Co(Dipc)₂]·7H₂O (Dipc=pyridine-2,6-dicarboxylic acid) has been synthe- sized and characterized by IR, elemental analysis, and X-ray diffraction. Crystal data: orthorhombic system with space group Pnna and unite cell parameters: a=2.0645(3)nm, b=1.3484(2)nm, c=0.8204(1)nm; V=2.2838(6)nm³, Z=4, D_cald=1.726 g·cm^-3, μ=1.193 mm^-1, F(000)=1212, Gof=1.045, Δρ=339～-348 e·nm^-3, the final R is 0.0295. In the molecule of the complex, Co(Ⅱ) ion is six-coordinate to form a dis-torted octahedron. The N atom and the carboxyl group of pyridine-2,6-dicarboxylic acid are coordinated with the central ions. One of the carboxyl groups of the pyridine-2,6-dicarboxylic acid connect K(Ⅰ) and Co(Ⅱ). The com- pound possesses approximate C₂ symmetry. The compounds form a three-dimensional network of infinite length connection with crystal waters, potassium ions and hydrogen bonds. The result of kinetics of thermal decomposition indicated that the compound decomposition takes place in two steps. CCDC: 207078.     

Synthesis, Crystal Structure, Thermal Stability and Luminescent Properties of a New 2D Zinc Complex

A new coordination polymer associated with zinc ion,[Zn(Tda)(bpp)] n (1,H 2 tda=thiophene-2,5-dicarboxylic acid,bpp=1,3-bis(4-pyridyl)propane),was prepared under solvothermal conditions,and characterized by single-crystal X-ray diffraction,elemental analysis and IR spectra.The complex belongs to monoclinic,space group P2 1 /c with a=9.8799(4),b=12.0430(6),c=15.4269(9),β=95.424(5) o,V=1827.33(16) 3,Z=4,D c=1.577 g/cm 3,S=1.074,μ=1.486 mm-1,F(000)=888,M r=433.80,R=0.0359 and wR=0.0968 for 2685 observed reflections (I > 2σ(Ⅰ)).Complex 1 displays an interesting 2D lattice structure.In 1,four coordinated zinc ions were bridged by Tda and bpp ligands to generate a (4,4) two-dimensional layer.The thermogravimetric analysis,powder X-ray diffraction (XRD) and luminescent properties for 1 also have been explored.     

Fe(III)与两种4-羟基吡啶二酸形成的配合物的合成与晶体结构

A iron(III) complex [Fe(2,6-HDA)(2,5-HDA)(H₂O)₂]·2.5H₂O (2,6-HDA=4-hydroxypyridine-2,6-dicarboxylic acid, 2,5-HAD=4-hydroxypyridine-2,5-dicarboxylic acid), has been hydrothermally synthesized and characterized by elemental analysis, IR and single crystal X-ray diffraction. It belongs to monoclinic system, with space group C2/c, a=0.155 8(4) nm, b=0.215 8(5) nm, c=0.133 0(3) nm, β=125.468(3)°, V=3.641 1(15) nm³, Z=8. The geometry around iron(III) is a distorted pentagonal bipyramid. CCDC: 631130.     

Hydrothermal Synthesis and Crystal Structure of a Coordinated Polymer： [Ni（pda）（H2O）3]n （pda = Pyridine-2,3-dicarboxylate）

1 INTRODUCTIONThe design and synthesis of metal-organic coor- dinated polymer have attracted considerable atten- tion in recent years. The infinite networks construc- ted from transition metal complexes have intere- sting structures as well as potential applications as smart electronic, magnetic porous materials, cataly- sis, host-guest chemistry, and so on[1～4]. In the as- sembly and synthesis of polymer structures, the me- tal ions, bi- or multi-dentate ligand, solvent and the ratio of …     

2,2-二苯基-2-羟基乙酸苯胺加合物的合成及其晶体结构

合成了2,2-二苯基-2-羟基乙酸苯胺加合物(1),其结构经UV,IR和X-射线单晶衍射仪表征。1的分子式为C34H31NO6,分子量为549.60,晶体属于三斜晶系,P1空间群,晶胞系数为:a=8.646(16),b=13.357(2),c=14.117(3),α=69.685(3)°,β=77.593(3)°,γ=71.748(3)°,V=1.441 3(5)nm3,Z=2,Dr=1.266 mg.cm-3,F(000)=580,μ(Mo Kα)=0.087 mm-1。结构由直接法解出,最终偏离因子为R1=0.054 6,wR=0.123 3。1通过分子间氢键连接形成超分子化合物。     

[Ni(Phen)3][Ni(DPC)2]·11.5H2O的合成及其晶体结构

以吡啶-2,6-二甲酸(H2DPC)和1,10-邻菲咯啉(Phen)为原料,首次合成了配合物[Ni(Phen)3][Ni(DPC)2].11.5H2O(1,C50H53N8Ni2O19.5),其结构经元素分析和X-射线表征。结果表明,1属单斜晶系,空间群为C2/c,晶胞参数为:a=29.863(3),b=14.971(2),c=24.638(3),β=104.800(10)°,V=10650(2)3,Z=8,S=0.883,Dc=1.491g.cm-3,μ=0.792mm-1,F(000)=4968。1由配阳离子和配阴离子通过静电引力结合而成,两个中心镍离子的配位多面体都是变形的八面体构型。     

3-羟基-1-金刚烷甲酸钴邻菲略啉配合物的合成和晶体结构

以硫酸钻、邻菲咯啉（phen）和3-羟基-1-金刚烷甲酸（HOC10H14COOH）为原料,合成了配合物[Co（HOG10H14COO）2（H2O）（phen）]·H2O;利用元素分析、红外光谱、热重分析对产物进行了表征,采用单晶X射线衍射方法测定了其晶体结构．结果表明,所合成的配合物C34H42N2O8Co属于单斜晶系,空间群C2／c,a=2．69798（7）nm,b=1．14319（3）nm,c=2．29092（6）nm,β=120．498（1）°,V665．63,F（000）=2808,Dc=1．452g·cm^-3,μ（Mo-Kα）=0．765mm^-1;R1=0.0805,wR2=0.2209,其通过氢键和π-π堆积作用相结合,形成稳定的二维超分子结构．     

Synthesis and Crystal Structure of Palladium(Ⅱ) Complex with 2,2''-Bipyridine-3,3''-dicarboxylic Acid

The title complex Pd(H2BDA)Cl2(2DMSO (C16H14Cl2N2O6PdS2, H2BDA = 2,2'- bipyridine-3,3'-dicarboxylic acid) has been synthesized and characterized by IR spectra, elemental analysis and 1H NMR spectra. Its structure was determined by single-crystal X-ray diffraction analysis. The complex crystallizes in the monoclinic system, space group P21/c with a = 1.3604(6), b = 1.2606(6), c = 1.3521(6) nm, β = 103.677(7)°, V = 2.2530(17) nm3, Mr = 571.75, Z = 4, Dc = 1.686 g/cm3, μ = 1.280 mm-1, F(000) = 1136, R = 0.0405 and wR = 0.0908. The complex presents a planar quadrangle arrangement and is assembled via hydrogen bonds.     

Hydrothermal Synthesis and Crystal Structure of a New One-dimensional Nickel(Ⅱ) Complex with 2-Pyridinecarboxyic Acid and 4,4''-Bipyridine Ligands

A new metal-organic coordination polymer [Ni[(2-pya)2(4,4'-bipy)]n.6nH2O (2-pya = 2-pyridinecarboxylic acid, 4,4'-bipy = 4,4'-pyridine) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in tetragonal, space group I41/a with a = b = 22.5642(19), c =10.7118(18) (A°), V = 5453.8(11) (A°)3, C22H28N4NiO10, Mr= 567.19, Dc=1.382 g/cm3, μ(MoKα) =0.769 mm-1, F(000)= 2368, Z = 8, the final R = 0.0572 and wR = 0.1254 for 1401 observed reflections (I> 2σ(I)). It exhibits a one-dimensional chain-like structure by mixed ligands of 2-pyridinedicarboxylic acid and 4,4'-pyridine.     

含羧酸配体的鼓形有机锡氧簇合物：六聚苯基锡氧3-吲哚丁酸酯的合成及晶体结构

利用Ph3SnOH和3-吲哚丁酸以1：1摩尔比反应，合成了新型含羧酸配体的鼓形 有机锡氧簇合物：六聚苯基锡氧3-吲哚西酸酯。通过元素分析、红外光谱和X射线 单晶衍射对其结构进行了表征。测试结果表明：该化合物为三斜晶系，空间群P1， a=1.1722(6),b=1.5694（8）nm，c=1.7227(9)nm，α=116.251（8）°，β=100. 854（10）°，γ=95.606（9）°，Z=1，V=2.732(3)nm^3，Dc=1.554g·cm^-3，μ =1.420mm^-1，F(000)=1276，R=0.0630，ωR=0.0762。晶体结构中，六配位的锡原 子呈畸变的八面体构型。     

铀-钾异核配位聚合物的合成及晶体结构

在水热反应条件下合成了1种新颖的U(Ⅵ)-K异核配位聚合物[UO2K2(pdc)2(H2O)3]n(H2pdc=吡啶-2,6-二羧酸),通过元素分析、红外、紫外光谱及热重对该配合物进行了表征。单晶结构表明:配合物属于单斜晶系,C2/c空间群;晶胞参数分别为a=1.888 5(6)nm,b=1.490 0(5)nm,c=0.740 2(2)nm,β=111.104(10)°。中心铀及钾原子通过2个氮原子和6个氧原子与吡啶-2,6-二羧酸配体结合。不同的[UO2K2(pdc)2].3H2O单元通过氧原子桥联组成三维链状配位聚合物。配位聚合物中存在π…π相互作用及氢键作用。