Crystal structure and standard molar enthalpy of formation of ethylenediamine dilauroleate (C12H24O2)2C2N2H8(s)

The crystal structure of ethylenediamine dilauroleate was determined by X-ray crystallography. A thermochemical cycle was designed in accordance with Hess law. The enthalpy change of the synthesis reaction of ethylenediamine dilauroleate was determined to be $ \Updelta_{{\text{r}}} H_{{\text{m}}}^{\Uptheta } $ Δ r H m Θ  = ?(49.07 ± 0.11) kJ mol^?1 by an isoperibol solution–reaction calorimeter. The standard molar enthalpy of formation of the title compound was calculated to be $ \Updelta_{\text{f}} H_{\text{m}}^{\Uptheta } $ Δ f H m Θ  = ?(38.78 ± 0.43) kJ mol^?1 by the designed thermochemical cycle, the enthalpies of dissolution and other auxiliary thermodynamic quantities.     

配合物Nd(C7H7N2O2)3(H2O)3的合成及其晶体结构

用水热法合成了3,5-二氨基苯甲酸与Nd(Ⅲ)的配合物Nd(C7H7N2O2)3(H2O)3(1),其结构经IR,元素分析和X-射线单晶衍射仪表征。1为单核结构,属六方晶系,R3空间群,晶胞参数:a=1.887 29(18)nm,b=1.887 29(18)nm,c=0.603 53(12)nm,β=90,°γ=120°,V=1.861 7(4)nm3,Z=3,μ=2.154 mm-1,Dc=1.744 g.cm-3,R1=0.014 3,wR2=0.033 2。1中Nd(Ⅲ)与来自3个3,5-二氨基苯甲酸的6个氧原子及3个配位水的氧原子进行配位,形成9配位化合物。     

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.     

三元混合配合物Cu(C10H8N2O3)·(C5H5N)·(H2O)的合成和晶体结构

The novel copper(Ⅱ) complex with 2-oxo-propionic acid benzoyl hydrazone and pyridine ligands, Cu(C₁₀H₈N₂O₃)·(C₅H₅N)·(H₂O) (C₁₀H₈N₂O₃^2- is the dinegative ion of 2-oxo-propionicacid benzoyl hydrazone), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex was determined by single crystal X-ray diffraction technique. Complex crystallized in the triclinic space group P1 with a = 0.729 08(10) nm, b= 1.020 01(14) nm, c= 1.126 28(15) nm, α = 71.644(2) °, β = 80.437(2) °, γ = 89.160(2)°, V= 0.78328(18) nm³, Z= 2, D_c= 1.547 Mg·m^-3, μ(MoKα) = 1.417 mm^-1, F(000) = 374. The final R₁ = 0.030 6, wR₂= 0.084 2 for 2 992 observed reflections [I≥2σ(I)] out of 3357 unique reflections. In this complex, copper(Ⅱ) ion is square-pyramidally coordinated by two oxygen atoms and one nitrogen atom of tridentate C₁₀H₈N₂O₃^2- ligand, one nitrogen atom of the pyridine ligand, and one oxygen atom of water molecule with the oxygen atom of water molecule locating at the apical position. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 222656.     

Heat Capacities and Thermodynamic Properties of Fenpropathrin (C22H23O3N)

The heat capacities of fenpropathrin in the temperature range from 80 to 400 K were measured with a precise automatic adiabatic calorimeter. The fenpropathrin sample was prepared with the purity of 0.9916 mole fraction. A solid—liquid fusion phase transition was observed in the experimental temperature range. The melting point, T_m, enthalpy and entropy of fusion, _fusH_m, _fusS_m, were determined to be 322.48±0.01 K, 18.57±0.29 kJ mol^–1 and 57.59±1.01 J mol^–1 K^–1, respectively. The thermodynamic functions of fenpropathrin, H_(T)—H_(298.15), S_(T)—S_(298.15) and G_(T)—G_(298.15), were reported with a temperature interval of 5 K. The TG analysis under the heating rate of 10 K min^–1 confirmed that the thermal decomposition of the sample starts at ca. 450 K and terminates at ca. 575 K. The maximum decomposition rate was obtained at 558 K. The purity of the sample was determined by a fractional melting method.This revised version was published online in November 2005 with corrections to the Cover Date.     

(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,Crystal Structures and Properties of Three New Complexes [Ni（C9N2O2H7）2（CH3OH）2],[Zn（C9N2O2H7）2（H2O）2] and [Cd（C9N2O2H7）2（CH3OH）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/m3,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/m3,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).     

Heat capacity and thermodynamic properties of 2,4-dichlorobenzaldehyde (C7H4Cl2O)

Heat capacities of 2,4-dichlorobenzaldehyde have been measured with a high-precision automatic adiabatic calorimeter over the temperature range from (79 to 371) K. The melting temperature, molar enthalpy, and entropy of fusion were determined by the heat capacity measurements to be (347.24 ± 0.13) K, (20468 ± 19) J · mol⁻¹, and (58.94 ± 0.04) J · K⁻¹ · mol⁻¹, respectively. The melting temperatures for the sample and the absolutely pure compound have been obtained from fractional melting experiments to be (347.230 and 347.619) K, respectively, and the chemical purity of the sample was calculated to be 0.9921 mol fraction according to the Van't Hoff equation. Moreover, the solid-to-liquid phase transition of the substance was further investigated by using DSC technique. The results obtained from the heat capacity measurements were in agreement with those from the DSC analysis.