Synthesis and Crystal Structure of [VO2（C17H11N3O2） ] [VO （C4H13N3）（C6H5N3O） ]（C2H5OH）

The reaction of VO（acac）2 with 2-hydroxyl-1-naphthaldehyde isonicotinyl hydrazone and amines （ethylenediamine or diethylenetriamine） in CH3OH yields crystals of novel vanadium compounds characterized by IR, NMR spectroscopic methods and X-ray single-crystal structure determination. Two different vanadium units exist in the crystal cell of [VO2（C17H11N3O2）][VO- （C4H13N3）（C6H5N3O）]（C2H5OH） which crystallizes in the triclinic system, space group P1 with a = 8.0104（17）, b = 13.898（3）, c = 14.955（3）A, α = 89.103（4）, β = 79.551（4）, γ = 78.352（4）°, V = 1603.3（6）A^3, Mr = 723.54, Dc = 1.499 g/cm^3, Z = 2, λ（MoKα） = 0.71073 ]A,μ= 0.644 mm^-1, F（000） = 748, the final R = 0.0547 and wR = 0.0997 for 8920 observed reflections with I 〉 2σ（I）. According to structure analysis, two different molecules are arranged in the lattice and the two vanadium atoms adopt octahedral and square pyramidal coordination geometries, respectively. The interactions between DNA and vanadium complexes have been investigated by UV-Vis absorption spectro- photometry.     

配合物(n-Bu)2Sn(C10H8N2O4)(C2H5OH)的合成和晶体结构

以2-羰基丙酸水杨酰腙作为配体与二正丁基氧化锡(Ⅳ)在苯/乙醇混合溶剂中反应, 合成了新型配合物(n-Bu)2Sn(C10H8N2O4)(C2H5OH)(C10H8N2O42为2-羰基丙酸水杨酰腙负二价离子)。用单晶X-射线衍射分析法测定了该配合物的晶体结构。晶体属四方晶系, I41/a空间群, 晶胞参数a = 2.5113(7), b = 2.5113(7), c = 1.5062(6) nm, V = 9.499(5) nm3, Z = 16, Dc = 1.396 g/cm3, m(MoKa) = 1.105 mm1, F (000) = 4096。对于2499 (I >2s(I))个可观测点, 最终可靠因子R = 0.0349, wR = 0.0793。在该配合物的分子结构中, 中心锡原子与3个O原子、1个N原子和2个C原子形成扭曲的八面体几何构型, 其中3个O原子和1个N原子为赤道配位原子, 而CSnC为配合物的轴。相邻配合物分子间因Sn…O的弱相互作用和分子间氢键的作用而以二聚体的结构形式存在。     

(C5H6N4O)(C5H5N4O)3(C5H4N4O)[Bi2Cl11]Cl2 as a simple and efficient catalyst in Biginelli reaction

A highly efficient and facile procedure for the one‐pot three‐component synthesis of 3,4‐dihydropyrimidin‐2‐(1H )ones/thiones from the one‐pot condensation of aldehyde, β‐dicarbonyl compound and urea/thiourea was developed. The methodology is applicable to a wide range of substrates with high yield in the presence of (C₅H₆N₄O)(C₅H₅N₄O)₃(C₅H₄N₄O)[Bi₂Cl₁₁]Cl₂. The complex is an air‐stable, environmentally friendly and recoverable catalyst and can efficiently catalyze the Biginelli reaction. The catalyst has high catalytic efficiency with low catalyst loading, and can be recycled ten times with only a small loss of activity.     

配合物[Mn(C13H8N2OBr)2(C5H5N)2]·3C5H5N的结构与磁性研究

The complex [Mn(C₁₃H₈N₂OBr)₂(C₅H₅N)₂]·3C₅H₅N has been synthesized and characterized by X-Ray diffraction, IR and variable temperature (～10 to ～278K) magnetic susceptibility. X-Ray diffraction result for the single crystal shows that the crystal belongs to monoclinic, space group P2₁/c, a=1.0969(3)nm, b=2.0903(5)nm, c=2.0481(6)nm, β=97.366(6), V=4.657(2)nm³, Z=4, D_c=1.47g·cm^-3。