Optical properties for N,N’-bis (lnaphyhly)N,N’-diphenyl-1,1’-biphenyl-4,4’-diamine and tris (8-hydroxyquinolinato) aluminum in organic light emitting devices

The optical properties of N,N’-bis (Inaphthyl)N,N’-diphenyl-1,1’-biphenyl-4,4’-diamine (NPB) and tris (8-hydroxyquinolinato) aluminum (Alq3) organic materials used as hole transport and electron transport layers in organic light-emitting devices (OLED) have been investigated. The NPB and Alq3 layers were prepared using thermal evaporation method. The results show that the energy band gap of Alq3 is thickness independence while the energy band gap of NPB decreases with the increasing of sample thickness. For the case of photoluminescence the Alq3 with thickness of 84 nm shows the highest relative intensity peak at 510 nm.

IR, 1H NMR, Electronic Properties and Conductivity Studies of N1 ,N4-Bis（Diphme）Benzene-l,4-Diamine Chloride Zirconium （IV） [{（Ar）2NC6H5N（Ar）2}ZrCl4] （Ar = C6H5）

A range of new compounds such as N1,N4-bis（diphenylmethlene）benzene-l,4-diamine zirconium （IV） chloride [{（Ar）2NC6HsN（Ar）z}ZrCl4] （Ar = C6H5） complex counting the chelating amine and chloride in position trans have been prepared. Well-defined NI,N4-bis（diphenylmethlene）benzene-l,4-diamine zirconium （IV） chloride [{（Ar）2NC6H5N（Ar）2}ZrCl4] （Ar = C6H5） was obtained by stoichiometric addition of {（Ar）2NC6H5N（Ar）2} （Ar = C6H5） and {ZrC14} in ethanol at reflex temperature. IR, 1H NMR, electronic properties using hyperchem program study has been improved for this compound such as bond distance, and this compound was also defined as electric conductivity which proves to be useful for conductively compound.

Synthesis and Characterization of a Novel Copoly(aryl ether ketone) Containing 4, 4'-Biphenyl-bis[4-phthalazin-1(2H)-one] Moiety

A new monomer of 4, 4-biphenyl-bis[4-phthalazin-1(2H)-one] was synthesized from biphenyl and phthalic anhydride, and a novel copoly(aryl ether ketone) (PPEK) was synthesized from 2, 2-bis(4-hydroxyphenyl)-propane (BPA), 4, 4'-biphenyl-bis-[4-phthalazin-1(2H)-one], 4, 4- difluorodiphenylketone (DFK). The monomer and copolymer were characterized by FT-IR and 1H-NMR. DSC and TGA were used to the novel polymer.

UPLC-MS/MS法测定槲寄生抗肿瘤成分1,7-bis(4-hydroxyphenyl)-1,4-heptadien-3-one的含量

目的建立超高效液相色谱-串联质谱法(UPLC/MS/MS)测定槲寄生中具有抗肿瘤活性的新化合物1,7-bis(4-hydroxyphenyl)-1,4-heptadien-3-one(BHPHD)的含量,并通过多因素方差分析比较产地与寄主对药材抗肿瘤成分含量的影响。方法以Thermo Hypersil GOLD C18(50 mm×2.1 mm,1.9μm)为分离色谱柱,乙腈-体积分数0.1%甲酸水溶液为流动相,流速0.2 m L·min-1,梯度洗脱,质谱检测器,电喷雾正离子,多反应监测模式,监测离子对m/z 295.09→106.99。结果BHPHD在质量浓度为0.050~2.5 mg·L-1内线性关系良好,精密度、重复性、稳定性试验的RSD均≤3.5%,平均加样回收率(n=9)为97.2%(RSD=1.6%)。结论该方法可满足定量要求。多因素方差分析表明槲寄生中BHPHD的含量受产地影响较大(P<0.01),受寄主影响不大。

A Three-dimensional Porous Metal-organic Framework Based on Cyano Unit and 1,4-Bis(1,2,4-triazol-1-yl)butane(btb):{[Cu_8(btb)_2(CN)_8].3H_2O}_n

The title coordination polymer 1,{[Cu8（btb）2（CN）8].3H2O}n（btb = 1,4-bis（1,2,4-triazol-1-yl）butane）,has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex 1 crystallizes in monoclinic,space group C2/c with a = 1.2938（3）,b = 1.9422（5）,c = 0.9406（2） nm,β = 121.891（4）°,V = 2.0066（9） nm3,C24H30Cu8N20O3,Mr = 1155.00,Dc = 1.912 g/cm3,μ（MoKα） = 4.209 mm？1,F（000） = 1140,GOF = 1.184,Z = 2,the final R = 0.0634 and wR = 0.1503 for I 2σ（I）.In complex 1,one-dimensional CuCN zigzag chains are linked by triazolyl groups of btb ligands to form two-dimensional networks,which are further bridged by 1,4-butyl moieties of btb ligands to fabricate a three-dimensional order framework,in which one-dimensional ellipsoid-like channels are observed.

Synthesis,Structural Characterization and Properties of Bis(1,5-diamino-1Htetrazolium)3,3'-bis(nitramino)-4,4'-azofurazan

An energetic salt of bis（l,5-diamino-lH-tetrazolium）3,3＂-bis（nitramino）-4, 4x-azo- furazan （C6H10N2206） was synthesized with the total yield of 61.7% by using 3,4-diaminofurazan （DAF） as the starting material. The structure of the title compound was confirmed by NMR, IR, elemental analysis and single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group P21/c with a = 10.739（2）, b = 6.4765（12）, c = 14.138（3） A, fl= 108.787（3）°, V= 930.9（3） A3, Z = 1, Mr= 486.36, Dc = 1.735 g.cm3, μ= 0.15 mm-1, F（000） = 496, R = 0.042 and wR = 0.121. The thermal stability was analyzed by subsequently differential scanning calorimetry （DSC）. And the enthalpy of formation and detonation was calculated theoretically, showing the first decomposition temperature was 142.1℃, the enthalpy of formation was 1614.23 kJ.mol1 and the detonation velocity and detonation pressure were 8.781 km.s-1 and 30.7 GPa, respectively.

Synthesis Characterization Non-isothermal Kinetics of the Thermal Decomposition and Redox Properties Derived from Copper(Ⅱ) Binuclear Coordination Compound of 1,4-Bis-(1'-Phenyl-3'-Methyl-5'-Pyrazolone-4')-1,4-Butanedione

The paper reports the synthetic procedure and character of Copper(II) binuclearcoordination compound of 1,4-bis-(1'-phenyl-3'-methyl-5'-pyrazolone Thenon-isothermal kinetics of thermal decomposition of the complex has been stUdied from the TG-DTGcurves by means of the Achar et al. and Coats-Redfern methods,the most probab1e kinetic equation canbe expressed as dofdtrAe -E / RT * l /(2Q).The corresponding kinetic compensation effect expressions arefound to be lnuA=0. 1794E+0. 1689.The non-isothermal thermal decomposition process of the complex isone-dimensional diffusion.But electrochemical studies of the complex(Cu2L'2)from cyclic voltamrnetriccurves by means of powder microelectrodes technique'',shows one two-electron irreversible process.

Syntheses and Characterization of Two Novel Copper(II) Malonate Complexes Functionalized with 3,3’-Bis(pyrazolyl)pentane and 4,4’-Trimethylenedipyridine

Two novel copper complexes (1,2) with N,O-donor ligands were synthesized by reaction of copper(II) malonates with 3,3’-bis(pyrazolyl)pentane and 4,4’-trimethylenedipyridine in methanol at moderate temperature. These compounds were characterized by elemental analysis, UV-VIS, IR spectroscopies and powder X-ray diffraction analyses. Compound (1) melts at higher temperature (202°C) than compound (2) (100°C). The IR spectra showed typical vibrations related to C=N and C=C, characteristic of pyrazolyl and pyridine ligands.

联苯吡菌胺关键中间体3′,4′-二氯-5-氟-1,1′-联苯-2-胺的合成

为获得联苯吡菌胺关键中间体3′,4′-二氯-5-氟-1,1′-联苯-2-胺的适合工业化生产工艺路线,对其合成工艺进行了优化。以3,4-二氯溴苯和2-溴-4-氟苯胺为原料,经格氏和Suzuki偶联2步反应合成了3′,4′-二氯-5-氟-1,1′-联苯-2-胺,其结构经1H NMR、MS表征确证,并对合成条件进行了优化。优化条件下,3′,4′-二氯-5-氟-1,1′-联苯2-胺合成总收率61.9%,纯度98%。该工艺成本低,收率高,具有工业化生产前景。

Solubility and metastable zone width measurement of 3,4-bis (3-nitrofurazan-4-yl) furoxan (DNTF) in ethanol + water

The solubility and supersolubility of 3,4-bis(3-nitrofurazan-4-yl)furoxan(DNTF) in ethanol + water at different operation were determined by laser monitoring system under atmospheric pressure to study the metastable zone width(MSZW). The modified Apelblat equation was adopted to correlate the experimental solubility data, and the correlation result showed perfect consistent with the experimental data. The standard dissolution enthalpy, standard dissolution entropy and Gibbs energy were calculated according to the experimental solubility data. The effect of the cooling rate, stirring rate, temperature and the concentration of ethanol + water on the MSZW was studied. It was found that the MSZW of DNTF increased with the increasing cooling rate, decreasing temperature, decreasing stirring rate and decreasing ratio of water. And the apparent nucleation order of DNTF in ethanol + water was calculated by the relationship between the cooling rate and the MSZW.

Synthesis and Structural Characterization of 2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol

2,3-Bis（hydroxymethyl）-2,3-dinitro-1,4-butanediol（C6H12N2O8） was synthesized by condensation,cyclization,oxidative dimerization and deketalization of nitromethane with a total yield of 42.4%.The structure of the title compound was characterized by 1H NMR,13C NMR,FT-IR,elementary analysis,and X-ray single-crystal diffraction analysis,which reveals that the title compound crystallizes in triclinic,space group P with a = 0.6324（2）,b = 0.6454（3）,c = 0.7062（3） nm,α= 111.550（4）,β= 95.505（4）,γ= 113.395（4）°,V = 0.23595（16） nm3,Z = 1,Mr = 240.18,Dc = 1.690 g·cm-3,μ = 0.159 mm-1,F（000） = 126,R = 0.0304 and wR = 0.0907.

A New Two-dimensional Zinc Coordination Polymer Constructed by 1,3-Bis(4-pyridyl)-propane and Terephthalate: Synthesis and Crystal Structure

A new zinc coordination polymer, [Zn2（bpp）（tpa）2H2O] 1 （bpp=1,3-bis（4-pyridyl）-propane and tpa=terephthalate） has been hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. X-ray crystal structure analysis reveals that complex 1 crystallizes in monoclinic, space group P2/c with a=18.348（2）, b=10.9080（14）, c=13.7924（18）, β=98.156（2）°, V=2732.5（6）3 , Z=4, C29H24N2O9Zn2 , Mr=675.24, Z=4, F（000）=1376, Dc=1.641 mg/m3 , μ=1.815 mm-1 , the final R=0.0443 and wR=0.0769 for 2715 observed reflections （I〉2σ（I））. The title complex exhibits a two-dimensional （4, 4） sheet structure which is further stacked through face-to-face π-π interactions between the monodentately coordinated pyridine ring of bpp ligand and the phenyl ring of terephthalate ligand to form a 3-dimensional supramolecular structure. Thermogravimetric analyses show that the host framework of the complex is thermally stable up to ca. 400 ℃.

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 mm1,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 coπmplex.

Synthesis and Crystal Structure of a One-dimensional Mn(Ⅱ) Coordination Polymer with 1,3-bis(4-pyridyl)propane

A new 1D zigzag chain coordination polymer, { [Mn（bpp）（bac）2]·（CHaCN）}n 1 （bpp = 1,3-bis（4-pyridyl）propane, Hbac = benzoylacetone）, has been synthesized and characterized by FT-IR spectroscopy, thermal analysis and X-ray single-crystal diffraction. In the molecular structure, all Mn atoms locate in an octahedral geometry. The guest CH3CN molecules are included in the 1D channels of the 3D packing structure of 1. Crystal data： C35H35MnNaO4, Mr = 616.60, monoclinic, space group P211c, a = 17.691（4）, b = 18,955（4）, c = 9.712（6） A, β = 93.91（3）°, V = 3249.31（1） A^3, Z = 4, Dc = 1.260 g/cm^3, F（000） = 1292, 20max = 54.9°, μ = 0.447 mm^-1, the final S = 1.020, R = 0.0693 and wR = 0.1497.

Synthesis and Crystal Structure of 3,3'-Bis(5-(N-(4-hydroxylphenyl)imidomethyl)- pyrrol-2-yl)pentane·2CH_3OH

3,3＇-Bis（5-（N-（4-hydroxylphenyl）imidomethyl）pyrrol-2-yl）pentane 1 has been synthesized and characterized. The crystal of its methanol complex, 1·（CH3OH）2, belongs to the orthorhombic system, space group Pccn with a = 18.094（2）, b = 11.6890（16）, c = 13.3629（19） , V = 2826.3（7） 3, Z = 8, C14.5H18N2O2, Mr = 252.31, Dc = 1.186 g/cm3, F（000） = 1080 and μ（MoKα） = 0.080 mm-1. The final R = 0.0662 and wR = 0.1801 for 1908 observed reflections with I 2σ（I）, and R = 0.0800 and wR = 0.1948 for all reflections. In the solid state, bridged by included methanol molecules, the molecules of compound 1 form interpenetrated grid structure through N–H···O and O–H···O hydrogen bonds.

Catalytic Kinetic on the Thermal Decomposition of Ammonium Perchlorate with a New Energetic Complex Based on 3,5-Bis(3-pyridyl)-1H-1,2,4-triazole

A new energetic complex,[Co（3,3？-Hbpt）（Htm）]·H_2O（1,3,3？-Hbpt = 3,5-bis（3-pyridyl）-1H-1,2,4-triazole and H_3tm = trimesic acid）,has been synthesized by hydrothermal reactions and characterized by single-crystal X-ray diffraction,elementary analysis,IR spectroscopy,thermogravimetric analysis and X-ray powder diffraction. Single-crystal X-ray diffraction indicates that the complex belongs to triclinic system,space group P 1 with a = 10.0911（1）,b = 10.2573（1）,c = 10.6393（1） ？,α = 103.793（2）,β = 101.041（2）,γ = 107.918（3）o,V = 974.9（2） ？~3,Z = 2,D_c = 1.732 g·cm-3,μ = 0.941 mm^（-1）,M_r = 508.31,F（000） = 518,the final R = 0.0523 and wR = 0.0935 with I 〉 2σ（I）. In the title complex,Co（Ⅱ） ions are connected by Htm2-anions generating 1D ladder-like chains which are linked by 3,3？-Hbpt to form 1D cages. In addition,the thermal decomposition of ammonium perchlorate（AP） with complex 1 was explored by differential scanning calorimetry（DSC）. AP is completely decomposed in a shorter time in the presence of complex 1,and the decomposition heat of the mixture is 2.531 kJ·g^（-1）,significantly higher than that of pure AP. By Kissinger＇s method,the ratio of Ea/ln（A） is 11.05 for the mixture,which indicates that complex 1 shows good catalytic activity toward the AP decomposition.

An efficient synthesis of 2,2-bis(1H-indol-3-yl)-2H-acenaphthen-1-one catalyzed by recyclable solid superacid SO_4^(2-)/TiO_2 under grinding condition

An efficient synthesis of symmetrical 2,2-bis（1H-indol-3-yl）-2H-acenaphthen-1-one is achieved via a reaction of acenaphthe-nequinone and indoles catalyzed by solid superacid SO4^2-/TiO2 under solvent-free conditions at room temperature by grinding, which provides an efficient route to the synthesis of symmetrical 2,2-bis（1H-indol-3-yl）-2H-acenaphthen-1-one.This procedure offers several advantages including solvent-free conditions,excellent yields of products,simple work-up as well as reuse of catalysts which makes it a useful and attractive protocol for the synthesis of these compounds.

One-dimensional Zigzag Chain Composed of HgI_2 Unit and 2,5-Bis(4-pyridyl)-1,3,4-thiadiazole:[HgI_2(C_(12)H_8N_4S)]

The title compound, [HgI2（C12H8N4S）], has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/n with a = 14.086（2）, b = 6.0365（6）, c = 20.286（2）°A,β= 108.818（5）°, V = 1632.7（3）°A^3, Mr = 694.67, Z = 4, D, = 2.826 g/cm^3,μ= 13.331 mm^-1, F（000） = 1240, S = 1.108, the final R = 0.0438 and wR = 0.0934 for 3085 observed reflections （I〉 2σ（I））. The Hg（Ⅱ） atom is coordinated by two 2,5-bis（4-pyridyl）-1,3,4-thiadiazole （L） molecules and two iodine anions in a distorted tetrahedral coordination geometry. Mercury atoms are linked by the organic ligands to form a one-dimensional zigzag chain. It is noteworthy that such 1D zigzag chains are extended into a two-dimensional double layer framework through I…I interactions

Synthesis,Crystal Structure and Theoretical Calculations of a Cadmium Complex Containing 3-Hydroxybenzoic Acid and 1,4-Bis(imidazol-1-yl)-butane

A new complex [Cd（hba）2（bib）]n·nH2O（1,Hhba = 3-hydroxybenzoic acid,bib = 1,4-bis（imidazol-1-yl）-butane） has been hydrothermally synthesized and characterized by elemental analysis,IR spectrum,thermogravimetric analysis,fluorescence spectrum,and singlecrystal X-ray diffraction.Yellow crystal crystallizes in the orthorhombic system,space group Pbca with a = 16.220（5）,b = 14.980（5）,c = 20.521（5） ？,V = 4986（3） ？~3,C（24）H（26）CdN4O7,Mr = 594.89,Dc = 1.585 g/cm^3,μ（Mo Kα） = 0.927 mm^（-1）,F（000） = 2416,Z = 8,the final R = 0.0242 and w R = 0.0589 for 4076 observed reflections（I 〉 2s（I））.In 1,the Cd（Ⅱ） ion takes a six-coordination mode,and bib ligand bridges adjacent Cd（Ⅱ） ions to generate 1D zigzag chains; these neighboring chains are connected by O–H···O hydrogen bonding interactions,producing a 2D folded layered structure.Furthermore,by O–H···O hydrogen bonding between layers and layers,a 3D supramolecular architecture is formed.In addition,we analyzed Natural Bond Orbital（NBO） in using the PBE0/LANL2 DZ method built in Gaussian 03 Program.The calculation results indicated obvious covalent interaction between the coordinated atoms and Cd（Ⅱ） ion.

Syntheses, Structures, and Properties of Three Coordination Polymers: [Cd_2(bpp)_(1.5)(Hbpp)(phen)_2]_n, [Mn_3(Htptc)_2(phen)_2(H_2O)_2]_n, and {[Cu(btc)_(0.5)(1,4-bib)]·2H_2O}_n

Hydrothermal reactions of three aromatic polycarboxylic acids and the transitional metal cations in the presence of phen and 1,4-bib afford three new coordination polymers： [Cd2（bpp）1.5（Hbpp）（phen）2]n （1）, [Mn3（Htptc）2（phen）2（H2O）2]n （2）, and {[Cu（btc）0.5（1,4- bib）]·2H2O}n（3） （H2bpp = 2,6-bis（4＇-carboxyphenyl）-4-phenylpyridine, H4tptc = terphenyl-2,5,2＇,5＇-tetracar- boxylic acid, H4btc =biphenyl-2,2＇,4,4＇-tetracarboxylic acid, phen =1,10-phenanthroline, and 1,4-bib = 1,4-bis（1H-imidazol-1-yl）benzene）. Their structures have been determined by single- crystal X-ray diffraction analyses, elemental analyses, IR spectra, and powder X-ray diffraction （PXRD） analyses. In compound 1, the CdII cations are linked by bpp2- to form one ladder structure, based on which a 3D network is constructed with the help of non-covalent interactions. The topology of 2 is a 3D （3,4,5）-connected framework with the Point Schl？fli symbol of （42.6）2（43.62.8）（45.64.8）2. Compound 3 shows an unprecedented 3D （4,4）-connected framework with the Point Schl？fli symbol of （64.82）2（65.8）. Moreover, the luminescent property of 1 has been investigated.