Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]^(2+)·[SbCl_5]^(2-)}_2

A new supramolecular compound, { [2-（2-pyridyl）benzimidazoleH2]2＋.[SBC15]2-}2, was synthesized by the hydrothermal reaction of o-diaminobenzene, 2-pyridinecarboxylie acid and SbCl3 in 1：1 HC1 solution, and characterized by chemical analysis, elemental analysis, IR spectra, thermogravimetfic analysis and fluorescence spectra. The crystal structure was deter- mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P211c, with a = 16.0397（13）, b = 14.3189（12）, c = 15.6370（13） A, β = 105.8980（10）°, V = 3454.0（5） A3, Z = 4, C24H22Cl10N6Sb2, Mr = 992.48, Dc = 1.909 g/cm3,/z = 2.366 mm-1, S = 1.010, F（000） = 1920, R = 0.0254 and wR = 0.0555. The coordination anion, [SbCl5]2- which is a distorted tetragonal pyramid, is composed by coordinating action with Sb3＋ ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2- form a biquaternion ring structure through the secondary bonding of Sb...Cl. Moreover, the compound adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-（2-pyridyl）benzimidazole divalent cations. The title compound also shows good fluorescent behaviors.

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Novel Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]_2·[BiCl_6]·Cl}

A novel supramolecular compound,{[2-（2-pyridyl）benzimidazoleH2]2·[BiCl6]·Cl},was synthesized by the hydrothermal reaction of o-phenylenediamine and α-pyridinecarboxylic acid with BiCl3 in 6.0 mol·L-1 HCl solution,and characterized by elemental analysis,IR,X-ray single-crystal diffraction and photoluminescence spectroscopy.The crystal （C24H22N6Cl7Bi,Mr= 851.61） belongs to the triclinic system,space group P1 with a =7.2887（18）,b =9.548（2）,c= 12.469（3）,α=85.306（4）,β=82.814（4）,γ=71.349（4）°,Z=1,V=814.9（3）3,Dc=1.735 g/cm3,μ（MoKα）=6.007 mm-1,F（000）=410,R=0.0307 and wR=0.0787.The bismuth ion and six chlorine ions construct a distorted octahedral configuration.The three-dimensional supramolecular network is built from electrostatic attractions,hydrogen bonds and π-π interaction between the BiCl6 anion,Cl anion and [2-（2-pyridyl）benzimidazoleH2] cation.The photoluminescence spectroscopy study shows that the title compound has a blue fluorescent emission at 450 nm in the solid state.

Synthesis and Crystal Structure of 4-Oxo-1,2,4-triazino[4,5-a]benzimidazole

The title compound 4-oxo-1,2,4-triazino[4,5-a]benzimidazole（C9H6N4O,Mr = 186.18） has been synthesized and structurally characterized by IR,NMR and single-crystal X-ray diffraction. The crystal belongs to monoclinic,space group P21/c,with a = 9.1530（18） ,b = 7.2260（14）,c = 12.604（3） ,β = 106.92（3） ,V = 797.5（3）A^3,Z = 4,Dc = 1.551 g/cm^3,λ（MoKa） = 0.71073,F（000） = 384,μ（MoKa） = 0.109 mm^-1,the final R = 0.0632 and wR = 0.1095. A total of 1444 unique reflections were collected,of which 767 with I 〉 2σ（I） were observed. The structure of the title compound is planar. In packing,the molecules are intersected to each other to form chains along three dimensions,together by intermolecular N-H…O and C-H…N hydrogen bonds. The whole structure is further stabilized by π…π interaction between two adjacent tricyclic ring systems,with the centroid-to-centroid distance of 3.369（4） A.

Synthesis,Crystal Structure and Biological Activity of 2-[(Pyridin-2-yl)methylthio]-1H-benzimidazole Derivatives

In order to discover the novel anti-tumor agents, a series of 2-[（pyridin-2-yl）methylthio]-1 H-benzimidazole derivatives were designed and synthesized, and the structures were characterized by IR, MS, and proton NMR. 2-[（3,4-Dimethoxypyridin-2-yl）methylthio]-1 Hbenzimidazole was investigated with X-ray crystallography, and the molecule is in orthorhombic system, space group P212121, with a = 9.1828（16）, b = 11.625（2）, c = 13.463（2） ？, Z = 4, R = 0.0231 and wR = 0.0596. The antitumor activities of target compounds were evaluated against human liver cancer cell line HepG2, and human liver normal cell line HL7702 using MTT assay. The target compounds have demonstrated weak or moderate anti-tumor activity against HepG2, while all the target compounds exhibit no cytotoxic effects on HL7702.

Synthesis and Structure of L-Aspartato- nickel(II) Complex with Benzimidazole

The title complex Ni(C4H5NO4)(C7H6N2)31.75(H2O) (C25H26.5N7NiO5.75, Mr = 575.74) has been prepared and its crystal structure was determined by X-ray diffraction method. The crystal of this chiral complex belongs to monoclinic, space group P21 with a = 13.208(1), b = 10.741(1), c = 19.398(1) ? b = 104.39(1)o, V = 2665.8(4) 3, Z = 4, Dc = 1.435 g/cm3, m(MoKa) = 0.780 mm-1 and F(000) = 1198. The final R = 0.0504 and wR = 0.1267 for 9159 observed reflections (I > 2s(I)), and R = 0.065 and wR = 0.1299 for 11006 independent reflections. The complex assumes a distorted octa- hedral coordinate geometry formed by one aspartate dianion and three benzimidazole ligands. The aspartate chelates to the Ni atom as a tridentate ligand. The lattice water molecules are hydrogen- bonded to the Ni complex molecule.

Crystal Structure and Electronic Structure of a Luminescent Compound 2-(2-Pyridyl) Benzimidazole

The crystal structure of 2-(2-pyridyl) benzimidazole was determined by single- crystal X-ray diffraction at 193(2) K. It crystallizes in orthorhombic system, space group Pbca with unit cell constants a = 10.6204(7), b = 10.1407(4), c = 18.6327(8) , Z = 8, V = 2006.7(2) 3, Dc = 1.292 g/cm3, F(000) = 816 and m(MoK) = 0.081 mm-1. The structure was refined to R = 0.0317 and wR = 0.0454 for 795 observed reflections with I > 2s(I). In the solid state, it has an emission maximum at 369 nm, while in solution (DMSO), the maximum excitation is at 372 nm. Quantum chemistry calculation was performed by the method of density functional theory. Theoretical results show that atom N is the reactive site when coordinating with a metal, and the electronic structure of the title compound presents excellent carrier transport properties.

Syntheses,Crystal Structures and Properties of Three New Complexes [Ni(C_9N_2O_2H_7)_2(CH_3OH)_2],[Zn(C_9N_2O_2H_7)_2(H_2O)_2] and [Cd(C_9N_2O_2H_7)_2(CH_3OH)_2]

Three novel metal-organic complexes with formulas [Ni（C9N2O2H7）2（CH3OH）2]（1）,[Zn（C9N2O2H7）2（H2O）2]（2） and [Cd（C9N2O2H7）2（CH3OH）2]（3） were synthesized by the reactions of Ni,Zn and Cd salts with ethyl 2-benzimidazolylacetate under hydrothermal conditions or layering technique,and characterized by single-crystal X-ray diffraction analysis,IR spec-troscopy,solid-state luminescent properties and thermogravimetric（TG） analysis.The crystal data for these three complexes are as follows：for 1,monoclinic,space group P21/c,a = 9.384（3）,b = 9.634（3）,c = 11.292（3） ,β = 95.787（5）°,V = 1015.7（5） 3,Z = 2,F（000） = 492,Dc = 1.547 Kg/m3,μ = 1.002 mm-1,the final R = 0.0451 and wR = 0.0900 for 1833 observed reflections with Ⅰ 〉 2σ（Ⅰ）;for 2,orthorhombic,space group Pbca,a = 10.031（4）,b = 10.379（4）,c = 17.525（7）,V = 1824.6（12） 3,Z = 4,F（000） = 928,Dc = 1.645 Kg/m^3,μ = 1.392 mm-1,the final R = 0.0452 and wR = 0.0996 for 1661 observed reflections with Ⅰ 〉 2σ（Ⅰ）;for 3,monoclinic,space group P21/c,a = 9.9114（13）,b =10.4852（15）,c = 10.4120（14） ,β = 108.453（5）°,V = 1026.4（2） 3,Z = 2,F（000） = 532,Dc = 1.705 Kg/m^3,μ = 1.110 mm-1,the final R = 0.0322 and wR = 0.0805 for 1822 observed reflections with Ⅰ 〉 2σ（Ⅰ）.In the three complexes,the ethyl 2-benzimidazolylacetate shows the same chelating mode,and the adjacent units are interlinked into a two-dimensional layer through hydrogen-bonds（O-H…O,N-H…O）.

离子化合物｛[2-(3′-pyridyl)benzimidazoleH_2]^(2+)·[SbCl_4]^-·Cl^-｝_4的水热合成、晶体结构及抑菌活性

A new ionic compound ｛[2-(3′-pyridyl)benzimidazoleH2]2+·[SbCl4]-·Cl-｝4 was synthesized by the hy- drothermal reaction of o-diaminobenzene, nicotinic acid with SbCl3 in 1∶1 HCl solution. The structure was charac- terized by chemical analysis, elemental analysis and IR patterns. The single crystal structure was determined by X-ray single crystal diffraction. It crystallizes in monoclinic system, space group P21/n with a=2.107 9(4) nm, b= 1.482 0(3) nm, c=2.113 4(4) nm, β=93.44(3)°, Z=4, V=6.590(2) nm3, Dc=2.001 g·cm-3, μ=2.480 mm-1, F(000)= 3840, R1=0.0468, wR2=0.1163. The single crystal structure indicates that the four chlorines coordinated to the antimony atom forms a distorted triangle bipyramid configuration together with the lone electron pair on the Sb atom. The [SbCl4]- to 2-(3′-pyridyl)benzimidazole cation and Cl- by weak interaction forms the ionic crystal. It has been proved that the title compound has antibacterial activity. CCDC: 283824.

A 2D Wavy Parquet Architecture Based on the Biphenyl-3,3',4,4'-tetracarboxylic Acid and Bis(2-benzimidazole)alkanes Ligands

A double-T-shaped ligand （H4BPTC） and bis（2-benzimidazole）alkanes as the spacers have been firstly used to direct the assembly of a 2D coordination polymer with wavy parquet network topology, [Zn（BPTC）0.5（H2C2EIm）（H2O）]n （1, C24H18ZnN4O5, Mr = 507.79, H4BPTC = biphenyl-3,3＇,4,4＇-tetracarboxylic acid, H2C2EIm = 2,2＇-（1,2-ethanediyl）-bis（1H-benzi- midazole）, which was determined by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/n with a = 1.1844（5）, b = 1.4019（5）, c = 1.4026（5） nm, β = 108.359（5）°, V = 2.2104（15） nm3, Z = 4, Dc = 1.526 g/cm3, μ（MoKα） = 1.156 mm-1, F（000） = 1040, S = 1.038, the final R = 0.0427 and wR = 0.0793 for 3834 reflections with I 2σ（I）. The compound units are linked through BPTC ligands into a wavilness parquet 2D layer and further connected into a 3D framework via π-π packing interactions between the adjacent H2C2EIm ligands and weak N-H…O hydrogen bonding between uncoordinated carboxylate and the nitrogen atoms of H2C2EIm as well as the free water molecules.

苯并咪唑类化合物一步法合成及表征

采用对甲氧基苯甲醛、对羟基苯甲醛和邻苯二胺直接关环合成了 1 (对甲氧基苄基 ) 2 (对甲氧基苯基 ) -苯并咪唑、1 (对羟基苄基 ) 2 (对羟基苯基 ) -苯并咪唑化合物 .通过元素分析、IR、核磁分析对它们进行了表征 ,并培养了 1 (对甲氧基苄基 ) 2 (对甲氧基苯基 ) -苯并咪唑化合物晶体 .该晶体经X射线衍射确定为正交晶系 ,空间群Pna2 ( 1) ,a =2 0 194( 7)nm ,b =1 5 65 7( 4 )nm ,c =0 5 498( 1)nm ,α =90° ,β =90° ,γ =90° ,V =1 73 83 ( 8)nm3 ,Z =4,Mr=3 44 40 ,Dc=1 3 16g/cm3 ,μ =0 85cm-1,F( 0 0 0 ) =72 8.

微波催化新型杂环基苯并咪唑杀菌剂的合成、表征及活性测定

以邻苯二胺及相应羧酸为原料,经环化、二茂铁磺酰化,合成了4种未见文献报道的二茂铁磺酰基苯并咪唑衍生物,经元素分析、MS、1H NMR测试技术确证结构。通过X射线衍射,测定了化合物4b的晶体结构,该晶体属单斜晶系,空间群P2(1)/c。晶胞参数:a=0.983 45(6)nm,b=1.702 37(11)nm,c=1.180 96(7)nm,α=90°,β=100.998(4)°,γ=90°,V=1.144 3(2)nm3,Z=4,F(000)=1 744,Mr=443.30,Dc=1.517 g/cm3,R1=0.098 3,wR2=0.110 1。通过琼脂稀释法初步测定了目标化合物4a～4d的杀菌活性,并与商品化的苯并咪唑杀菌剂麦穗宁进行对照试验。结果表明,化合物4a～4d具有良好的杀菌活性,其中化合物4d杀菌活性最高,对5个被测菌种的EC50在17.12～37.11 mg/L。

2,6-二(2-苯并咪唑基)吡啶与稀土苦味酸盐配合物的合成、晶体结构及荧光性质研究

合成了稀土苦味酸盐(pic)与配体2,6-二(2-苯并咪唑基)吡啶(L)的配合物,通过元素分析、红外光谱及电子光谱对配体及配合物进行了表征,并用X射线单晶衍射测定了配合物[CeL2(pic)2](pic)?(CH3OH)3的晶体结构.配合物属于三斜晶系,空间群为P-1,晶胞参数a=1.3795(3)nm,b=2.1292(5)nm,c=2.5651(6)nm,α=105.847(3)°,β=100.150(3)°,γ=107.893(3)°,Z=2,R=0.0519,wR=0.1255.晶体中一个不对称单元内有两个结晶学上独立的分子,这两个分子的构型基本相同,中心Ce3+均与两个三齿配位的配体及两个双齿配位的苦味酸根配位,配位数为10.中心Ce3+的配位多面体为变形双帽四方反棱柱,两个分子之间以π-π堆积连接,生成一个非中心对称的二聚体.整个晶体则是由这些二聚体以分子间氢键作用连接成三维网状超分子结构.室温下,在紫外光激发下Eu(III)配合物固体和溶液均表现出中心离子的特征荧光发射.

萘甲基苯并咪唑衍生物的合成、表征及其杀菌活性

以1萘乙酸和2萘乙酸为原料,在微波辐射下合成了相应的萘甲基苯并咪唑,经二茂铁磺酰化等步骤,合成了2种未见报道的萘甲基二茂铁磺酰基苯并咪唑衍生物。经元素分析、质谱、核磁共振确证结构。通过X射线衍射,测定了化合物2a的晶体结构。化合物2a为三斜晶系,空间群P1,晶胞参数:a=0.89055(10)nm,b=0.97034(10)nm,c=1.4610(2)nm,α=101.542(2)°,β=95.811(2)°,γ=109.780(10)°,V=1.1443(2)nm3,Z=2,F(000)=526,Mr=507.39,Dc=1.473Mg/m3,μ=1.016mm-1,R1=0.0386,wR2=0.0979。对5种农作物病菌的杀菌活性优于市售50%多菌灵可湿性粉剂。

N,N′-二羧甲基-2-甲基苯并咪唑内鎓盐的合成及晶体结构

以2-甲基苯并咪唑为原料,合成了一个新型的苯并咪唑二羧酸衍生物,基结构通过IR,1HNMR,元素分析和X-射线单晶衍射法确定。X射线衍射单晶结构分析表明,固态时标题化合物通过分子间氢键形成一维无限链状结构,这些一维无限链状结构又通过链与链间的苯并咪唑环的π-π堆积作用形成二维结构。标题化合物的晶体属单斜晶系,P21/c空间群;Mr:568.54,a=19.821(3),b=7,.4501(11),c=20.093(3),β=116.479(3),°v=2655.8(3)3,z=4,Dc=1.422 mg.m-3,F(000)=1200,最终偏离因子R=0.0675,wR=0.2187。

二(2-苯并咪唑亚甲基)胺配合物的合成、晶体结构、活性和量子化学研究

合成了[二(2-苯并咪唑亚甲基)胺][咪唑]合Cu(Ⅱ)Zn(Ⅱ)Cu(Ⅱ)高氯酸盐配合物C_(57)H_(57)N_(21)Cu_2Zn(ClO_4)_6·6[(CH_3)_2NCHO],并进行了元素分析、红外和紫外表征,用X射线衍射的方法测定了晶体结构。

(±)-1-[(2-羟基-5-甲基苯基)(苯基)甲基]-2-吡啶苯并咪唑的合成及晶体结构

Hydroxy 5 methylphenyl)(phenyl)methyl] 2 pyridylbenzimidazole was synthesized and its crystal structure was determined by X ray four cycle diffraction method. The crystal belongs to monoclinic, space group P2 1 /c , with the crystal cell parameters: a =1.351 4(5) nm, b =0.965 9(6) nm, c =1.674 0(3) nm, β =110.2 7(2)°, V =2.049 7(14) nm 3, Z=4, D c=1.269 g/cm 3, R 1= 0.057 5 . The analyses of crystal structure show that the chain structure is formed by intermolecular H bond. [WT5HZ]

二（2—苯并咪唑亚甲基）胺合Zn（Ⅱ）配合物晶体和电子结构研究及生物活性测定

合成了二(2-苯并咪唑亚甲基)胺合Zn(Ⅱ)高氯酸盐配合物[C16H15N5Zn@(C1O4)2@3H2O和C32H30N10Zn@(ClO4)2@C2H5OH],进行了元素分析、红外和紫外表征.对后者采用X射线方法测定了晶体结构,并采用G94W程序进行了量子化学计算.利用邻苯三酚自氧化法测定了所合成配合物的生物活性.

新型桥连双锌配合物的合成和结构

合成了二 ( 2 苯并咪唑亚甲基 )胺及其副产物 [2 ,5 二 (苯并咪唑亚甲基 )环二肽 ]的混合配体与Zn(Ⅱ )的双核超氧化物歧化酶模型化合物 .进行了元素分析、紫外和红外表征 ;对配合物采用X射线衍射方法测定了晶体结构 ,并采用G94W程序对副产物 [2 ,5 二 (苯并咪唑亚甲基 )环二肽 ]进行了量子化学计算 .

Zn(Ⅱ)与氯苯基苯并咪唑配合物的合成、表征和晶体结构

The title complex [ZnL 2Cl 2]·C 2H 5OH (M=639.70;L=2 (O chlorophenyl)benzimidazole) was prepared and characterized by elemental analysis,IR and molar conductivity measurement.The analysis of its single crystal x ray diffraction was carried out to obtain the crystal data:monoclinic,space group P2 1/n,a=1.1612(3),b=1.9339(4),c=1.3369(3)nm,β=107.88(2)°,V=2.8572(11)nm 3,Z=4,D c=1.487kg·dm -3 ,μ=1.263mm -1 ,F(OOO)=1304,the final R=0.0462,wR=0.1016,(Δ/σ) max =0.001,S=0.884.It was showed that the Zinc(Ⅱ) cation is the central ion of a distorted tetrahedral coordination with two imidazole nitrogen atoms and two chlorine ions in the tetrahedral sites.Structural changes in ligands of complex were discussed.

离子化合物[2,6-bis(Benzimidazol-2-yl)pyridineH_2]^(2+)·[SbCl_5]^(2-)的合成、晶体结构及荧光性质

利用邻苯二胺、2,6-吡啶二甲酸与三氯化锑在盐酸溶液中经水热反应,合成了一种新的离子型化合物[2,6-bis(Benzimidazol-2-yl)pyridineH2]2+.[SbCl5]2-。通过化学分析、元素分析、热重分析、红外光谱及荧光光谱对结构和性质进行了表征,用X-射线单晶衍射测定了该化合物的晶体结构。化合物的晶体属三斜晶系,P1空间群。Sb3+与其周围5个氯离子配位,构成一个畸变四方锥构型[SbCl5]2-配位结构,2个配阴离子[SbCl5]2-之间通过Sb(1)…Cl(1)ii次级键形成四元环状结构,并与2,6-二(苯并咪唑-2′)吡啶两价阳离子,通过离子键及氢键形成三维网状离子化合物晶体。该化合物具有很好的荧光特性。