Synthesis and Crystal Structure of N-Benzyl-N＇-（2-pyridyl）urea and Its Mononuclear Cu（Ⅱ） Complex

A new ligand of N-benzyl-N＇-（2-pyridyl）urea L and its self-assembly product with CuCl2, [Cu（Ⅱ）LCl2]∞ 1, have been synthesized and structurally characterized by IR, 1H NMR and single-crystal X-ray diffraction analysis. In the structure of L, the urea groups adopt Z,E conformation to form dimers through intermolecular hydrogen bonds; while in complex 1, it assumes Z,Z conformation to fit for the coordination sphere of the Cu（Ⅱ） ions. The coordinated units are connected through intermolecular N-H...Cl hydrogen bonds to form an extended 2D framework. Finally, a 3D structure is obtained via π-π stacking interactions between pyridyl rings     

Synthesis and Crystal Structure of （5-Hydroxy-6-methoxybenzofuran- 3-yl）-（4-methoxyphenyl）methanone

Compound 1 (5-hydroxy-6-methoxybenzofuran-3-yl)(4-methoxyphenyl)methanone, C17H14O5 , as a potential anti-breast cancer agent has been synthesized under microwave irradiation, which was further converted to (5,6-dihydroxybenzofuran-3-yl)(4-methoxyphenyl)methanone (2). The compounds were characterized by MS and NMR spectra. Meanwhile, the crystal of 1 was obtained and determined by X-ray single-crystal diffraction. Crystal data: monoclinic system, space group P21/n, a=8.908(6), b=10.505(7), c=15.452(11), β=105.043(9)°, V=1396.4(16)3 , Z=4, F(000)=624, Dc=1.419 g/cm3 , μ=0.105 mm1, R=0.0513 and wR=0.1246 for 14459 independent reflections (Rint=0.0647) and 2488 observed ones (I>2σ(I)). Intermolecular O-H···O and π-π stacking interactions contributed to the stability of the structure.     

Synthesis and Crystal Structure of 4-（4,6-Dimethoxylpyrimidin-2-yl）- 3-thiourea Carboxylic Acid Ethyl Ester

4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data： C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309（3）, b = 0.67682（6）, c = 1.74237（19） nm, β = 114.744（3）°, V= 2.7106（5） nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F（000） = 1200, Z= 8, R= 0.0514 and wR= 0.1529.     

Synthesis and Crystal Structure of 4-(4,6-Dimethoxylpyrimidin-2-yl)-3-thiourea Carboxylic Acid Ethyl Ester

4-(4,6-Dimethoxyl-pyrimidin-2-yl)-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine,potassium thiocyanate and methyl chloroformate in ethyl acetate.Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamidc at room temperature.The crystal structure was determined by X-ray diffraction analysis.Crystallographic data:C10H14N4O4S,Mr=286.31,monoclinic,space group C2/c with a=2.5309(3),b=0.67682(6),c=1.74237(19)nm,β=114.744(3)°,V=2.7106(5)nm3,Dc=1.403 g/cm3,μ=0.225mm-1,F(000)=1200,Z=8,R=0.0514 and wR=0.1529.     

交联聚苯撑乙炔的的合成及其荧光特性

利用Sonogashira偶联反应,首次合成了溶解性好且为乙烯基封端的聚苯撑乙炔化合物（PPE）,通过。HNMR谱、IR光谱对其结构进行了表征．将其热固化后,通过紫外可见吸收光谱和荧光发射光谱分析,证明了PPE的交联能够在一定程度上消除分子链间的相互作用和π-π堆积效应．     

Novel Copper（Ⅱ） and Zinc（Ⅱ） 2-D Supramolecular Structures Based on Carboxylate and 1-Substitutedimidazole Mixed-ligands

Using the ligand bis(3-(1H-imidazol-1-yl)-1-phenylpropan-1-one) L, two novel com- plexes [CuL2(ph))]·H2O 1 and [ZnL2(tp)] 2 (ph = phthalic acid, tp = terephthalic acid) have been synthesized and their crystal structures were determined by single-crystal X-ray diffraction analysis. Crystal data for 1: triclinic, space group P1, a = 9.4300(17), b = 12.148(2), c = 13.721(2) , α = 109.620(2), β = 94.351(2), γ = 94.830(2)°, C32H30N4O7Cu, Mr = 646.14, V = 1466.2(4) 3, Z = 2, Dc = 1.464 g/cm3, μ(MoKα) = 0.801 mm-1, F(000) = 670, the final R = 0.0337 and wR = 0.0859 for 5122 observed reflections with I > 2σ(I). And those for 2: monoclinic, space group P2/n, a = 7.1866(11), b = 14.144(2), c = 14.407(2) , β = 101.427(2)°, C32H28N4O6Zn, Mr = 629.95, V = 1435.4(4) 3, Z = 2, Dc = 1.457 g/cm3, μ(MoKα) = 0.908 mm-1, F(000) = 652, the final R = 0.0438 and wR = 0.0821 for 2546 observed reflections with I > 2σ(I). In 1 and 2, ph or tp ligands bridge the six-coordinated copper(II) or four-coordinated zinc(II) ions forming 1D zigzag chains while L ligands act as the terminal monodentate ligand. It is noted that weak non-classical C–H···O plays the important and dominating roles in the formation of 2D supramolecular architectures of 1, but in 2 non-classical C–H···O and aromatic π-π stacking interactions are quite important and play dominant roles in the self-assembly of 2D supramolecular architectures.     

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…     

Synthesis and Crystal Structure of Dichlorobis(1-methylimidazoline-2(3H)-thione-S) Cobalt(II)

The reaction of anhydrous cobalt(II) dichloride with 1-methylimidazoline-2(3H)thione in dichloromethane solution gave the title complex, [Co(C4H6N2S)2Cl2]. X-ray single-crystal analysis revealed that the complex crystallizes in a monoclinic system, space group P21/c, a = 13.9707(10), b = 10.0435(7), c = 10.3910(6) (A), β = 91.181(3)o, V = 1457.70(17) (A)3, Z = 4, C8H12Cl2N4S2Co, Mr = 358.17, Dc = 1.632 g/cm3, μ = 1.813 mm-1, F(000) = 724, the final R = 0.0710 and wR = 0.1224 for 1549 observed reflections with I > 2((I). The Co atom is coordinated by two S atoms from two 1-methylimidazoline-2(3H)-thione ligands and two chloride ions in a slightly distorted tetrahedral geometry. The intramolecular classical hydrogen-bonding interactions involving chloride ions and N-H groups of the heterocyclic thione ligands are observed. The offset π-π stacking interactions between the imidazole rings of adjacent molecules with a face-to-face distance of 3.604 (A) are found in the packing diagram.     

Synthesis and Crystal Structure of a New Copper(II) Complex with 4-Cyanobenzoic Acid

1 INTRODUCTION Exploration on the syntheses and properties of car- boxylate complexes, especially aromatic carboxylate complexes, has always been a fascinating and chal- lenging research field for decades either in coor- dination chemistry or in functional materials[1, 2]. Cy- anobenzoic acid (Hcba) possessing two functional coordination groups should display structural diver- sities on the formation of complexes[3～15]. In particu- lar, the copper(II) carboxylate complexes bearing spe- …     

Eu(DBM)3qp和Eu(DBM)3pp的晶体结构及荧光性质对比研究

两种新型铕配合物Eu(DBM)₃qp(DBM=二苯甲酰甲烷,qp=喹喔啉并[2,3-i]-1,10-邻二氮杂菲)和Eu(DBM)_3pp(DBM=二苯甲酰甲烷,pp=吡嗪并[2,3-i]-1,10-邻二氮杂菲)的晶体结构均属单斜晶系,P2(1)/c空间群.中心铕离子分别与DBM配体的六个氧原子及第二配体的两个鳌合氮原子配位,形成八配位的扭曲四方反棱柱构型.两种配合物晶体中,每四个配合物分子的第二配体共轭平面相互平行,形成一种特殊的"块"状π-π堆积单元.在紫外光激发下两种配合物均表现为Eu³⁺的特征发射,由于第二配体能级的不同,Eu(DBM)_3pp的发射强度比Eu(DBM)_3qp高十几倍.     

Solvothermal Synthesis and Crystal Structure of a 1D Helical-chain Cobalt（II） Complex Containing （Quinolin-8-yloxy）acetate

The cobalt(II) complex with (quinolin-8-yloxy)acetate, [CoCl(C11H8NO3)]n (1), has been prepared via the solvothermal method and characterized by IR, elemental analysis, UV- Vis diffuse-reflection spectra and single-crystal X-ray diffraction analysis. Complex 1 is a novel carboxylate-bridged one-dimensional helical cobalt(II) polymer, and the Co(II) centre exhibits an approximately square pyramidal CoClNO3 coordination geometry. It crystallizes in monoclinic, space group P21/n, with a = 9.1594(10), b = 6.8864(7), c = 17.290(2) , β = 102.629(3)o, C11H8ClCoNO3, Mr = 296.56, V = 1064.2(2) 3, Z = 4, Dc = 1.851 g/cm3, F(000) = 596, μ = 1.856 mm-1, the final R = 0.0308 and wR = 0.0807. Interestingly, the chain complexes are assembled to form two-dimensional networks through intermolecular face-to-face π-π stacking interactions with the centroid-to-centroid distance of 3.559(1)  and the dihedral angle of 8.4(1)° between the aromatic rings.     

Synthesis and Structure of a Novel Macrocyclic Complex [Cd2(phen)4(phth)2]·4H2O

A novel complex [Cd2(phen)4(phth)2]·4H2O has been synthesized by the reaction of H2phth(phthalic acid) and phen(1,10-phenanthroline) with Cd(Ⅱ) in ethanol-water solution. X-ray crystal structure analysis shows it crystallizes in triclinic, space group P1 with a = 10.619(3), b =12.560(4), c = 12.651(4) A, α = 98.775(5), β = 109.035(5), γ = 113.576(5)°, C32H24CdN4O6, Mr=672.95, V= 1381.7(7) A3, Rint = 0.0358, Z= 2, Dc= 1.618 g/cm3, μ = 0.845 mm-1, -6 ≤h≤13, -15≤k ≤13, -15≤l≤14, F(000) = 680, S = 1.038, R = 0.0480 and wR = 0.0849 for 3992 observed reflections (I ＞ 2σ(Ⅰ)). Phth bridges Cd(Ⅱ) to form a macrocyclic compound, and a 2D supramolecular motif is formed through hydrogen bonds and π-π interaction.     

双齿甜菜碱衍生物大环及双环镉(Ⅱ)配位化合物的合成与晶体结构

利用甜菜碱衍生物1,5-二(4-羧基吡啶基)-N-甲基二乙胺(L)合成了两种镉(Ⅱ)的配位化合物[Cd2Cl4(H2O)2L2].2H2O和[Cd2(SCN)4(μ-H2O)L2]。用X-射线单晶衍射仪测定了配合物的单晶结构,并对它们进行了元素分析、红外光谱、1H NMR、热重等表征。结构分析表明,前者具有三十六元大环框架,而后者为双环结构。由于缺乏分子之间的强烈相互作用,弱相互作用决定了这两种化合物在晶格中的堆积模式:前者由相邻分子间的π-π和C-H…π相互作用而堆积形成二维砖墙的结构;后者由配位的SCN-阴离子通过S…S弱相互作用联接成一维链状结构。     

一维链状配位聚合物[Cd(N-MeIM)_2(SCN)_2]_n的结构表征和电化学性能研究(英文)

0 IntroductionThe rapid development in the area of polymericmetalorganic frameworks (MOFs) continues to producevarious structures with interesting compositions andtopologies[1￣5] , along with potential applications asfunctional solid materials for molecular selection, ionexchange, and catalysis[6￣10]. By the careful selectionand design of organic ligands, such as linear isothio-cyanate-based building blocks, a wide variety of solid-state supramolecular architectures have been con-structed[1…     

Synthesis,Crystal Structure and Characterization of a New Coordination Polymer from the Self-assembly of CoCl_2 Salt and Flexible Ligand 1,3-Bis（4-pyridyl）propane

A new 1D coordination polymer [Co(bpp)3Cl2(H2O)2]n 1 (bpp = 1,3-bis(4-pyridyl)-propane) was synthesized and characterized by elemental analysis,IR spectrum and single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system,space group Ibca with a = 16.569(9),b = 17.240(10),c = 27.087(16) ,V = 7738(8) 3,Z = 8,Dc = 1.306 g/cm3,Mr = 760.65,λ(MoKa) = 0.71073 ,μ = 0.623 mm1,F(000) = 3192,the final R = 0.0678 and wR = 0.2011. The Co(II) atom is coordinated in a slightly distorted octahedral CoN4Cl2 geometry by two Cl atoms in the axial positions,four N atoms from the two bridging bpp ligands and two pendant bpp ligands. The CoN4Cl2 octahedra are connected by the bridging bpp ligands to form a 1D neutral coordination polymer chain. The chains are linked by face-to-face π-π interactions between adjacent pendant bpp ligands to give rise to a 3D supramolecular architecture. The photoluminescent investigation indicates that the emission of 1 is attributed to ligand-centered emission. The variable-temperature magnetic susceptibility measurement shows weak antiferromagnetic behavior in the complex.     

Synthesis and electrochemical properties of a series of novel tetra(4-benzoyl)phenoxyphthalocyanine derivatives

A novel phthalocyanine,2,9(10),16(17),23(24)-tetra(4-benzoyl)phenoxyphthalocyanine,and its complexes with Zn(II),Cu(II),Co(II),and Ni(II) have been synthesized and characterized by a combination of elemental analysis,IR,1 H NMR,UV-vis spectroscopy and mass spectrometry.All of the materials are very soluble in common organic solvents such as dichloromethane,chloroform,tetrahydrofuran,N,N-dimethylformamide and dimethyl sulfoxide.The Q band wavelengths of the complexes decrease in the order:Zn > Cu > Ni > Co.Redox processes were observed at 1.06,0.74,0.51 and 0.98 V for the free phthalocyanine,at 0.72 and 1.04 V for the Co(II) complex,at 1.24,0.77,0.24,0.61 and 0.91 V for the Cu(II) complex,and at 0.74 and 1.20 V for the Ni(II) complex.The cyclic voltammograms of the phthalocyanine ring of the four species are similar,with reduction and oxidation couples each involving a one-electron transfer process.     

Determination of Dopamine Using 2-(4-Boronophenyl)quinoline-4-carboxylic Acids as Fluorescent Probes

The selective identification of dopamine is a significant issue because this compound is an important neurotransmitter closely related to Parkinson’s disease and other mental disorders. 2-(4-Boronophenyl)quinoline-4-carboxylic acid (PBAQA) has been previously reported as a water-soluble fluorescent probe for catechol. However, there are no significant differences in the binding constants between catechol and catecholamines, such as dopamine or levodopa. Here a series of bis-boronic acid compounds based on PBAQA were synthesized and the binding activities were characterized. As a representative compound, the binding constant of 4-(4-((3-(3-borono-4-chlorobenzamido)propyl)carbamoyl)quinolin-2-yl)boronic acid to dopamine is up to 10⁴?L?mol^?1 and much higher than previously reported boronic acid probes. Dopamine selectivity may be achieved by the variation of the substituents in the probe molecules. 4-(4-((3-(3-Borono-4-methoxybenzamido)propyl)carbamoyl)quinolin-2-yl)boronic acid has a stronger binding affinity to dopamine (K_a=5204?±?106?L?mol^?1) than catechol (K_a=2588?±?273?L?mol^?1) or levodopa (K_a=2383?±?273?L?mol^?1). This fluorescence response was used for determining dopamine in a range from 5?×?10^?5?mol?L^?1 to 5?×?10^?4?mol?L^?1 with a detection limit of 7.7?×?10^?6?mol?L^?1. This compound has been successfully used for the assay of dopamine in rabbit plasma, exhibiting excellent specificity. It is believed that synthesized compounds hold great promise as practical platforms to monitor dopamine levels.     

Effect of Solvent on the Morphology and Microstructure of Light Emitting Organogels

Summary: Self assembly of oligo(phenylene vinylene) based gelator is studied in three different solvents namely, trans-decahydronaphthalene (trans-decalin), benzene and benzyl alcohol. The morphology as well as the thermal properties are different for benzyl alcohol gel as compared to those gels in trans-decalin or benzene. X-ray diffraction studies indicate that in case of benzyl alcohol gel, the molecular organization is highly ordered with respect to the fibrils grown in other two solvents.     

(d-p)π共轭作用对簇合物Mo_2S_4(dtp)_2和Mo_3S_4(dtp)_4·Py电子光谱的影响

比较了含有配位不饱和过渡金属原子簇合物Mo_2S_4(dtp)_2,(Ⅰ)和Mo_3S_4(dtp)_4·Py,(Ⅱ)的紫外—可见电子吸收光谱实验数据和半经验的量子化学方法INDO计算得到的电子跃迁能,讨论了(d-p)π型共轭作用对其电子吸收光谱位移的影响。结果表明,过渡金属簇合物中电子吸收光谱位移,与有机共轭体系有着类似的变化规律,即随着共轭π键数目增加,π-π电子跃迁的吸收光谱红移。