New Supramolecular Complex Assembled through Hydrogen Bonds. Crystal Structure of Co(PMBP-tsc)_2 ·2DMF·2H_2O

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Synthesis and structure analysis of diammonium 3,5-dinitro-1,2,4-cyclopentanetrione

A new energetic ionic compound, diammonium 3,5-dinitro-1,2,4-cyclopentanetrione (DDCP), has been synthesized. It has been characterized by elemental analysis, IR, and single-crystal X-ray diffraction. The compound crystallizes in triclinic system, space group P1, a=4.485(1) ?, b=7.527(1) ?, c=13.367(1) ?, α=94.15(1)°, β=92.73(1)°, γ=101.75(1)°, V=439.72(11) ?³, Z=2, and D _calc=1.784 Mg m⁻³; R=0.0331, R _w=0.0892 for 1643 reflections with I>2σ(I). The entities of two ammonium cations and 3,5-dinitro-1,2,4-cyclopentanetrione anions are held by electrostatic forces and intermolecular hydrogen bonds. The bivalent anion exists as all kinds of resonance structures, which is in favor of stability of the anion. The thermal decomposition of title compound is studied by using DSC and TG-DTG techniques. The results show that the title compound has a higher enthalpy change and can evolve abundant gas products.     

Synthesis,structure and properties of an imidazolate bridged copper,zinc binuclear complex

A new imidazolate bridged Cu~(2+),Zn~(2+)binuclear complex[(dtma) CulmZn (dtma)]ClO_4·2.5H_2O taken as active site model for Cu,Zn-SOD has been synthesized and its crystal structuredetermined.All the bond lengths, bond angles and the distance between Cu and Zn atoms in Cu-Im-Zn core of the model complex are close to those in Cu,Zn-SOD.ESR parameters of the modelcomplex as a function of pH show that the imidazolate bridge is stable in pH range 10—12,and isbroken on Zn side at pH～9.With decreasing pH,the imidazole is released at pH～4 and the dtmaligand dissociates from the Cu containing fragment at pH～2.4.     

Synthesis and characterization of nitro-p-xylenes

In this paper we elected to nitrate p-xylene because this compound has only one mononitro- and trinitro- isomer. Trinitro-p-xylene was used as a starting material for the synthesis of other compounds in subsequent work. The mononitration of p-xylene can be easily carried out at 30 degrees C. Nitro-p-xylene is easily nitrated to dinitro-p-xylene at a temperature of 80 degrees C. The trinitro-p-xylene can be obtained at 120 degrees C. Single crystals of 2,3-dinitro-p-xylene and 2,3,5-trinitro-p-xylene were grown using the slow cooling method and we report the X-ray structure of the former. The thermal decomposition of the compounds was studied using differential scanning calorimetry (DSC) and thermogravimetry-derivative thermogravimetry (TG-DTG) techniques and FT-IR. The target compounds were also characterized by (1)H-NMR, (13)C-NMR and MS.     

Taibaihenryiin C的构型、构象及晶体结构

从太白山产的鄂西香茶菜中分离得到新骨架的二萜类化合物TaibaihenryiinC,对其进行X射线衍射晶体结构分析,确定其分子中各取代基的相对构型、环构象及晶体结构.研究表明,C-3位的羟基和C-11位的乙酰氧基以C-20位的甲基为参考均位于β位;分子中的A环为椅式构象,B,C环接近于船式构象,D环接近于信封式构象.特别是在D环中存在较大的扭转角,使D环中有内应力存在,这表明该化合物具有潜在的生理活性.TaibaihenryiinC的晶体结构属正交晶系,P2₁2₁2₁空间群,晶胞参数a=0.6162(1)nm,b=1.2730(1)nm,c=2.5193(3)nm,Z=4.在晶体中分子间通过C-3位的-OH氢与C-11位的乙酰氧基上的羰基氧形成分子间氢键,使分子在晶体中沿a轴呈螺旋结构排列.     

N、N′-二乙基-N、N′-二苯基脲的萃取性能和二硝酸二(N、N′-二乙基-N、N′-二苯基脲)合铀酰(Ⅱ)配合物的合成、结构研究

The extraction behavior of N,N′-diethyl-N,N′-dibenzenyl-urea (DEDBU) to Uranium(Ⅵ) and Thorium(Ⅳ) from nitric acid solution was studied by using xylene as diluent. The effects of aqueous HNO₃ concentration and ex-tractant concentration on the extraction distribution ratio of U(Ⅵ) and Th(Ⅳ) were studied, and the results show that the extraction behavior of the extractant to U(Ⅵ) is similar to tributyl phosphate (TBP), the solvation numbers for DEDBU and TBP are two, respectively. Under the experiment condition, the extractant does not show the extraction behavior to Th(Ⅳ), this result exhibits that the extractant has good application to separate U(Ⅵ) and Th(Ⅳ). The crystal structure of the complex UO₂(NO₃)₂[CH₂(CH₂)₂CONC₈H₁₇]₂ was determined by single crystal X-ray diffraction. Crystal data: C₂₄H₄₆N₄O₁₀U, triclinic, space group , a = 8.662(2)?, b= 10.07(2)?, c= 10.895(3)?, α = 103.77(2)°, β = 92.01(2)°, γ = 96.23(2)°, V= 915.7(4)?³, M_r = 934.78, Z= 1, D_c= 1.695 g·cm^-3, F(000) = 462, μ = 4.495mm-1, R= 0.0250, wR= 0.0591, observed reflec-tions 3566 (I>2σ(I)).The central uranyl ions is coordinated by six oxygen atoms, two of them are from the carbonyl groups of N,N′-diethyl-N,N′-dibenzenyl-urea molecules, and the other four are from two nitrate groups.     

Crystal and molecular structure of main adduct of benzaldoxime dehydrodimer and styrene

Three 1:1 adducts have been obtained by heating benzaldoxime dehydrodimer with styrene. The main product possesses the structure of bis-nitrone type. A radical addition mechanism is proposed.     

新型氰基桥联配位聚合物[Ni(en)2]2[Ni(CN)4]2·5H2O的合成、晶体结构和磁性质

分子组装在材料科学、催化和生物化学中具有潜在的应用前景,所以分子组装引起了化学、固体物理学和生物学等领域科学家们的普遍关注.分子组装常用的方法是使用具有配位能力的金属配合物作为建筑块与过渡金属阳离子反应.     

[Ni(CHZ)3](TNR).5H2O的制备、晶体结构和热分解机理

用2,4,6-三硝基间苯二酚(斯蒂芬酸, TNR)镍的水溶液和碳酰肼(CHZ, NH2NHCONHNH2)水溶液反应, 制备出配合物[Ni(CHZ)3](TNR).5H2O, 测定了其晶体结构, 并用 TG-DTG, DSC 和 IR技术研究了其热分解机理. 该晶体属三斜晶系, P空间群, 晶胞参数a＝1.045 40(10) nm, b＝1.167 1(2) nm, c＝1.227 8(2) nm, α＝109.190(10)°, β＝121.168(12)°, γ＝99.700(10)°, V＝1.261 3(3) nm3, Z＝2, Dc＝1.744 g/cm3, μ(Mo,Kα)＝0.873 mm-1, F(000)＝688, R＝0.041 9, Rw＝0.105 3. 在该配合物分子中, 碳酰肼为双齿配体, 由羰基O原子和1位N原子与Ni2+离子配位, 分子中共形成3个五元平面螯合环, 中心离子为六配位八面体结构. 该配合物在程序升温条件下, 分两步脱去所含结晶水, 第一步失去4个结晶水, 第二步失去1个结晶水, 在500 ℃时的最终分解产物为Ni2O3.     

{[Cd(NTO)2(CHZ)]·2H2O}n的合成、分子结构和热分解机理

通过3-硝基-1,2,4-三唑-5-酮(NTO)镉与碳酰肼(NH₂NHCONHNH₂,CHZ)反应制备出了新型配合物{[Cd(NTO)₂(CHZ)]·2H₂O}_n,研究了其分子结构和热分解机理。该配合物的晶体属正交晶系,Pbca空间群,晶体学参数:a=0.8623(1)nm,b=1.8259(4)nm,c=1.9997(3)nm