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.     

(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.     

Syntheses and Crystal Structures of Complexes [Cu(C14H8N3O4Br)](C4H9NO) and [Ni(C14H9N2O3Br)](C4H9NO)

The title compounds, Cu(L1)(C4H8NHO) and Ni(L2)(C4H8NHO) (H2L1 = 5-bro- mosalicylaldehyde-p-nitrobenzoylhydrazone, H2L2 = 5-bromosalicylaldehyde-p-hydroxybenzo- ylhydrazone), have been obtained and characterized by single-crystal X-ray diffraction. Complex 1 belongs to the triclinic system, space group P1 with a = 8.6960(2), b = 9.957(2), c = 11.878(2) , α = 73.36(3), β = 78.25(3), γ = 82.64(3)o, V = 962.1(3) 3, Mr = 512.81, Z = 2, F(000) = 514, Dc = 1.770 g/cm3, μ(MoKα) = 3.251, R = 0.0337 and wR = 0.0846. Complex 2 is of monoclinic, space group P21/c with a = 13.313(2), b = 8.2096(1), c = 21.890(3) , β = 125.737(3)o, V = 1941.9(4) 3, Mr = 478.97, Z = 4, F(000) = 968, Dc = 1.638 g/cm3, μ(MoKα) = 3.085, R = 0.0356 and wR = 0.0817. The ligands form a satisfactory N2O2 square plane around the metal centers in two compounds. Different patterns of hydrogen bonds are observed owing to the presence of different substituents on aromatic ring of the acylhydrazone Schiff bases. In complex 1, square-planar copper(II) complexes are linked by intermolecular hydrogen bonds leading to zigzag infinite chains. In complex 2, the metal complexes are linked via hydrogen bonds to form corrugated sheets in a staggered fashion; 3D channels along the b axis are constructed through other non-covalent interactions between the neighboring layers.     

吡嗪桥连异三核配合物的合成及晶体结构

Ag(Ⅰ)配合物的几何构型多变,最常见的是配位数为2的线性构型和配位数为4的四面体构型。前者如Ag(NH_3)_2~+及Ag(CN)_2,后者如[Ag(SC(CH_3)NH_2)_4]Cl、[(Ph_3)Ag(Cl)]和[(Ph_3MeP)_3Ag(BH_4]等。配位数为4的平面四方构型却罕见,只在当有一定刚性的四氮杂环十四烷和Ag(Ⅰ)生成配合物时才是平面四方构型。 本文报道一种新型异三核含银配合物的合成及其晶体结构,其中Ag是平面四方构型。     

(C26H40N2O4)[Ln(NO3)5H2O]的合成及其铕缔合物的晶体结构

合成了4个新型的稀土化合物(C₂₆H₄₀N₂O₄)[Ln(NO₃)₅H₂O](Ln=Pr,Nd,Sm,Eu),采用元素分析和红外光谱表征,用四圆衍射仪测定了其中(C₂₆H₄₀N₂O₄)[Eu(NO₃)₅H₂O]的晶体结构,属三斜晶系,P1空间群,晶胞参数:α=0.9100(4)nm,b=1.3560(3)nm,c=1.6463(4)nm;α=68.62(2)°,β=74.84(3)°,γ=87.50(2)°;Z=2.中心铕离子由5个硝酸根的10个氧原子和1个水分子中的氧原子配位,配位数是11.1,7,10,16-四氧-4,13-二氮杂-N,N'-二苄基环十八烷(N,N'-二苄基穴醚(2,2))未参与配位.     

Syntheses and Structures of the Hexacoordinated Antimony Complexes: Ph3(C2H4O2)Sb⋅⋅⋅DMSO, (3-FC6H4)3(C2H4O2)Sb⋅⋅⋅DMSO,and (4-MeC6H4)3(C6H4O2)Sb⋅⋅⋅DMSO

Russian Journal of Coordination Chemistry - Complexes Ph3(C2H4O2)Sb???DMSO (I), (3-FC6H4)3(C2H4O2)Sb???DMSO (II), and...     

Photoelectron spectroscopic and theoretical study of aromatics-Pb(m) anionic complexes (aromatics = C6H5, C5H4N, C4H3O, and C4H4N; m = 1-4): a comparative study

The reactions between lead vapored by laser ablation and different aromatic molecules (C6H6, C5H5N, C4H4O, or C4H5N) seeded in argon carrier gas were studied by a reflectron time-of-flight mass spectrometer (RTOF-MS) with a photoelectron spectrometer. The adiabatic electron affinities (EAs) of the dominant anionic products PbmC6H5(-), Pb(m)C5H4N(-) (m = 1-4) and Pb(m)C4H3 (-), Pb(m)C4H4N(-) (m = 1-3) dehydrogenated complexes are obtained from the photoelectron spectra with 308 and 193 nm photon, respectively. It is found that the EAs of Pb(m)C4H4N are higher than those of Pb(m)C6H5, Pb(m)C5H4N, and Pb(m)C4H3O with the same metal number m. The possible structures for Pb(m)C4H4N(-) complexes were calculated with density functional theory (DFT) and the most stable structure was confirmed. The adiabatic detachment energies for the most stable structure were in agreement with the experimental PES results. The calculated density of state (DOS) agrees with the experimental PES spectrum well. It was confirmed by the theoretical calculations that the C4H4N group bonds on lead clusters through the Pb-N sigma bond.     

Thermal behaviour and vibrational spectra of (NH4)3Ga(C2O4)3 · 3H2O and (NH4)3Al(C2O4)3 · 3H2O

The IR and Raman spectra and the thermal behaviour of the isomorphous compounds (NH₄)₃Ga(C₂O₄)₃·3H₂O and (NH₄)₃Al(C₂O₄)₃·3H₂O were investigated. Detailed stoichiometries, sustained by TG, DTA and IR spectroscopic analyses, were found in both cases. Different results, associated with the different polarizing powers of the metal cations, were obtained. The first evidence was found of the formation of basic gallium carbonates.