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911.
A novel trinuclear nickel(Ⅱ) complex [Ni3(bushz)2(Himdz)2(H2O)2]?2DMF (1, bushz=N-butylsalicylhydrazide, Himdz=imidazole, DMF=N,N-dimethyl-formamide) has been synthesized and characterized by X-ray single-crystal diffraction characterization. Complex 1 crystallizes in the monoclinic system, space group P21/c with a=7.706(7), b=14.882(6), c=18.639(6) , β=108.08(2)o, V=2032(1) 3, Dc=1.525 g/cm3, Mr=932.95, Z=2, F(000)=972, μ=1.442 mm-1, the final R=0.0359 and wR=0.0771. The three nickel(Ⅱ) atoms in 1 are arranged in a strictly linear structure and exhibit alternating square-planar and octahedral geometries. The complex is connected to form a supramolecule with an infinite three-dimensional network through intermolecular hydrogen bonds. The electrochemical studies reveal that redox of Ni3+/Ni2+ in the complex is a quasi-reversible process. The thermal stability of the title complex was also studied. 相似文献
912.
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. 相似文献
913.
Three isomeric metal-organic frameworks,[Cd2(X)(btc)(DMA)3]n(X = Cl(1),Br(2),I(3),H3btc =1,3,5-benzenetricarboxylic acid and DMA = N,Nˊ-dimethylacetamide),have been synthesized and characterized by elemental analysis,infrared spectra(IR),thermogravimetric(TG) analyses and single-crystal X-ray diffraction.Single-crystal X-ray analysis reveals that compounds 1–3 crystallize in the orthorhombic P212121 space group,and feature a three-dimensional(3D) extended framework containing dinuclear [Cd2(COO)3] units as the secondary building units(SBUs).Topological analysis reveals that compounds 1–3 can be simplified into a 3-connected srs topological network. 相似文献
914.
One binuclear sodium(Ⅰ) complex [Na2(2-benzoylbenzoato)4(Phen)2(H2O)2]·H2O has been synthesized with 2-benzoylbenzoic acid and 1,10-henanthroline as ligands. The crystal structure was determined by X-ray diffraction. The crystal belongs to the triclinic system with space group P , a = 1.08096(8), b = 1.09619(8), c = 1.09740(8) nm, α = 79.0600(1), β = 71.0450(1), γ = 62.0540(1)o, V = 1.08533(1) nm3, Dc = 1.421 g/cm3, Z = 2, F(000) = 484, GOOF = 1.036, the final R = 0.0363 and wR = 0.0961. The crystal structure shows that two neighboring sodium(Ⅰ) ions are linked together by two bridging water molecules, and each end position is coordinated with one 1,10-phenanthroline molecule and one 2-benzoylbenzoato to form a binuclear structure. Each sodium(Ⅰ) ion in the molecule is coordinated with five atoms to give a distorted trigonal bipyramid. The fluorescence property of the title complex is also discussed. 相似文献
915.
Indolocarbazole derivatives have been reported to be promising organic semicon- ductor candidates and electroluminescent (EL) materials. One novel indolocarbazole derivative, 2,8-acetyl-5,11-dihexyl-6,12-(di-p-tolyl)-5,11-indolo[3,2-b]carbazole (YK4), has been synthesized, and its crystal structure has also been carefully studied. YK4 is triclinic, space groups Pi with a = 9.409(5), b = 13.974(5), c = 15.488(5) A, α = 90.281(5), β = 105.456(5), Z= 93.728(5)°, M,. = 688.94, V= 1958.1(14) A3, Z = 2, Dc.= 1.168 g/cm-3,μ = 0.070 mm-1, F(000) = 740, Rint = 0.0475, R (I〉 20(/)) = 0.1146, wR (I〉 20(/)) = 0.2186, R(all data) = 0.2192 and wR (all data) = 0.2701. Like other indolo[3, 2-b]carbazole derivatives which were introduced in the 5- and 11-positions, the intermolecular short contacts are localized between the pendant groups and acetyl groups of the neighboring indolocarbazole molecules. The molecule of YK4 possesses poor face-to-face π-π stacking between two adjacent molecules in the crystal. The calculated bond lengths and bond angles of YK4 also proved the result of crystallography. 相似文献
916.
917.
918.
利用Nafion,石墨烯(GS)和纳米金(AuNs)的N,N-二甲基甲酰胺(DMF)分散液制备了一种新型纳米复合膜修饰碳糊电极(CPE),建立了一种测定扑热息痛(PCT)的新方法。采用扫描电镜(SCE)对修饰电极进行了表征;利用循环伏安法(CV)研究了PCT在修饰电极上的电化学行为。利用微分脉冲溶出伏安法(DPSV)优化了测定PCT的试验条件。结果表明:PCT在Nafion/GS/AuNs修饰电极上于0.43V处出现了一灵敏的氧化峰(Epa),其电极过程受扩散控制。同时利用氧化峰可以进行微量PCT的检测,其峰电流(ip)与PCT浓度(c)在0.5~10μmol/L和10~900μmol/L范围内均呈良好的线性关系,相关系数分别为0.9968和0.9973,检出限(S/N=3)为0.1μmol/L。复合膜修饰电极稳定性较好,可用于实际药品中扑热息痛的含量的快速检测。 相似文献
919.
凝胶渗透净化/液相色谱串联质谱法测定动物源肝脏中4种β-激动剂的残留量 总被引:1,自引:0,他引:1
采用凝胶渗透净化技术,建立了用高效液相色谱串联质谱法同时测定动物源肝脏中克伦特罗、沙丁胺醇、莱克多巴胺、特步它林残留量的方法。样品经β-葡萄糖苷酸酶水解后,用乙酸铵溶液提取,MCX固相萃取柱和全自动凝胶渗透净化色谱仪净化,采用选择离子监控模式(SIM)检测,内标法定量。克伦特罗在0.1~10 ng/mL、莱克多巴胺、沙丁胺醇、特布他林在1~100 ng/mL质量浓度范围内呈良好的线性关系,相关系数(r2)均大于0.999;方法的检出限和定量限分别在0.003~0.02μg/kg和0.009~0.06μg/kg之间,方法的回收率为94.7%~106.1%,相对标准偏差小于7.8%。适用于动物肝脏中克伦特罗、沙丁胺醇、莱克多巴胺、特步它林的确认和定量检测。 相似文献
920.
建立了以HPLC法对傣药-肾叶山蚂蝗甲醇提取物清除二苯基苦基肼自由基(DPPH.)能力的方法,通过实验得出最佳的色谱条件:色谱柱为AgilentEclipse XDB-C18(4.6×150 mm,5μm),流速为1.0 mL/min,检测波长517 nm,柱温箱温度为20℃,进样体积20.0μL,流动相为不同比例的甲醇和水的混合液。在此条件下测定了DPPH.的清除率为50%时抗氧化剂的质量浓度(IC50)值,肾叶山蚂蝗甲醇提取物的IC50为1.51 mg/mL。 相似文献