[Ba_2(H_2TNP)_2(OH)_2(H_2O)_2]·(CH_3CH_2OH)·2.5H_2O配合物的合成、结构表征和热分析(英文)

Preparation,Structure Characterizations and Thermal Analysis of [Ba_2(H_2TNP)_2(OH)_2(H_2O)_2]·(CH_3CH_2OH)·2.5H_2O Complex

将NaHCO3与三硝基间苯三酚分散于蒸馏水中,加热搅拌制备出3,5二羟基2,4,6三硝基苯酚钠溶液,再与硝酸钡水溶液反应合成了3,5二羟基2,4,6三硝基苯酚钡盐。在乙醇的水溶液中培养得到了配合物([Ba2(H2TNP)2(OH)2(H2O)2]·(CH3CH2OH)·2.5H2O(H2TNP:3,5二羟基2,4,6三硝基苯酚盐),其化学式为C14H21Ba2N6O25.5。对其进行了元素分析和红外表征,利用单晶分析测定了晶体结构,晶体属于四角形晶系,空间群为I4(1)/amd,晶体学数据为:a=19.911(3)nm,b=19.911(3)nm,c=13.265(3)nm,V=5259.0(15)nm3,Z=8,对1092个衍射点R=0.0335。分子结构由二个氧桥联钡的二聚体单元组成。每个Ba原子是10配位,配位的氧原子分别为:8个来自4分子H2TNP,一个来自一分子H2O,一个来自氢氧根离子。金属原子由氧桥连成网状结构,非配位的水分子和乙醇分子位于晶体的空穴中。用DSC,TGDTG和IR技术研究了标题物的热分解机理,在550℃,分解残渣主要为BaCO3。

The Ba2 （ H2 TNP） 2 （ OH ） 2 （ H2 O） 2 ] · （ CH3 CH2 OH ） · 2.5 H2O （ H2 TNP ： 3,5-dihydroxy-2,4,6-trinitrophenolate） complex was prepared by mixing barium nitrate solution and sodium H2TNP solution, which was obtained through the reaction of sodium bicarbonate and trinitrophloroglucinol. The molecular structure was characterized by using element analysis, IR analysis and X-ray diffraction. The complex 1 crystallizes in tetragonal system, space group I4 （ 1 ）/amd, with crystal parameters a = 19.911 （ 3 ） nm, b = 19.911 （ 3 ） nm, c = 13. 265 （ 3 ） nm, V = 5259.0 （ 15 ） nm^3, Z = 8, R = 0. 0335 with 1092 reflections. The structure consists of a barium dimmer unit held together by two oxygens bridging. Each Ba atom is 10-coordinated with eight oxygen atoms from four H2TNP, an oxygen atom from water molecule and a coordinated hydroxy ion. In complex the metal atoms are linked via oxygen bridges to infinite networks structure. Uncoordinating water molecules and ethanol molecules are present in the cavities of the crystal structure. The thermal decomposition of the complex is studied using differential scanning calorimetry （ DSC）, thermogravimetry-derivative thermogravimetry （TG-DTG） and IR techniques. The final residue is BaCO3 at 550 ℃.