三硝酸根二(N,N,N′,N′-四丁基丙二酰胺)合镨(Ⅲ)配合物的晶体结构及热分解性质  

Crystal Structure and Thermal Decomposition of Tris(nitrato)di(N,N,N′,N′-Tetrabutyl malonamide) Complex of Pr(Ⅲ)

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作  者:崔玉[1] 孙国新[1] 李业新[1] 张振伟[1] 孙思修[2] 

机构地区:[1]济南大学化学化工学院,济南250022 [2]山东大学化学化工学院,济南250100

出  处:《无机化学学报》2005年第11期1723-1726,共4页Chinese Journal of Inorganic Chemistry

基  金:国家自然科学基金(No.20301008);山东省自然科学基金(No.Q2003B01)资助课题。

摘  要:The crystal structure of species Pr(NO3)3·2TBMA (TBMA=N,N,N′,N′-tetrabutyl malonamide) has been determined by X-ray diffraction. The compound crystallizes in the triclinic system, P1 space group, a=1.318 5(18) nm, b=1.449(2) nm, c=1.494(2) nm, α=70.03(2)°, β=71.53(2)°, γ=83.75(2)°, V=2.546(6) nm3, Z=2, Mr=979.97, Dc=1.278 g·cm-3, F(000)=1 032, R1=0.054 7. In each molecule, the metal ion is 10-coordinate, being bonded to two nearly coplanar bidentate TBMA ligands and three bidentate nitrate ions, two of them located on each side of the plane defined by the TBMA ligands and the third one crossing the plane. The geometry can be best described in terms of pentagonal bipyramid with each bidentate nitrate occupying one site. The two coordinated C=O groups in TBMA are not parallel, the O(1)-C(1)...C(3)-O(2) and O(3)-C(20)...C(22)-O(4) torsion angles are 129.73° and -48.43° respectively. The absorption bands belonging to the coordinated carbonyl vibration split into two peaks at 1 577.96 and 1 608.43 cm-1 respectively, which is caused by the different environment. The thermal decomposition of the complex is in three steps. CCDC: 231276.The crystal structure of species Pr(NO3)3·2TBMA (TBMA=N,N,N′,N′-tetrabutyl malonamide) has been determined by X-ray diffraction. The compound crystallizes in the triclinic system, PI space group, a=1.318 5(18) nm. b=1.449(2) nm, c=1.494(2) nm, α=70.03(2)°,β=71.53(2)°,γ=83.75(2)°, V=2.546(6) nm^3, Z=2, Mr=979.97, Dc=1.278 g·cm^-3, F(000)=1032, R1=0.054 7. In each molecule, the metal ion is 10-coordinate, being bonded to two nearly coplanar bidentate TBMA ligands and three bidentate nitrate ions, two of them located on each side of the plane defined by the TBMA ligands and the third one crossing the plane. The geometry can be best described in terms of pentagonal bipyramid with each bidentate nitrate occupying one site. The two coordinated C=O groups in TBMA are not parallel, the O(1)-C(1)…C(3)-O(2) and O(3)-C(20)…C(22)-O(4)torsion angles are 129.73° and -48.43° respectively. The absorption bands belonging to the coordinated earbonyl vibration split into two peaks at 1 577.96 and 1 608.43 cm^-1 respectively, which is caused by the different environment. The thermal decomposition of the complex is in three steps. CCDC: 231276.

关 键 词:硝酸镨 N N N′ N′-四丁基丙二酰胺 晶体结陶 热分解 

分 类 号:O614.334[理学—无机化学]

 

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