A New Dinuclear Gadolinium Complex Constructed from p-Phenylenediamine-N,N,N′,N′-tetraacetic Acid and in situ Generated Oxalate  

作　　者：于方永 郝志峰 李海峰 胡升 

机构地区：[1]Faculty of Chemical Engineering and Light Industry,Guangdong University of Technology

出　　处：《Chinese Journal of Structural Chemistry》2012年第9期1315-1321,共7页结构化学（英文）

基　　金：the National Natural Science Foundation of China (No. 21001030 and 21101032);the Foundation for the Authors of Excellent Doctoral Dissertation of Guangdong Province (No. sybzzxm201048);the "211" Creative Project of Guangdong Province

摘　　要：Routine solution reaction of Gd3＋ and p-phenylenediamine-N,N,N′,N′-tetraacetic acid （p-PhDTA） yields a dinuclear complex [Gd2（ox）（p-PhDTA）2（H2O）10]·6H2O （ox = oxalate）, which was characterized by single-crystal X-ray diffraction （MoKα radiation, = 0.71073）, elemental analysis and IR. This complex crystallizes in the monoclinic system, space group P21/n with a = 10.2522（8）, b = 10.0053（8）, c = 23.8834（18）, = 99.1080（10）°, V = 2419.0（3）3, Z = 2, Mr = 1367.32, Dc = 1.877 g/cm3, F（000） = 1368, = 2.830 mm-1, the final R = 0.0337 and wR = 0.0794 for 4747 observed reflections （I 〉 2 （I））. The exo-tetradentate oxalate ligand, generated in situ from the oxidative coupling of methanol, is incorporated to construct a dinuclear Gd2（ox）2 unit decorated with p-PhDTA ligands on the two sides with a monodentate coordination mode. The dinuclear molecules are further connected by the lattice water molecules to form a three-dimen- sional hydrogen network.Routine solution reaction of Gd3＋ and p-phenylenediamine-N,N,N′,N′-tetraacetic acid （p-PhDTA） yields a dinuclear complex [Gd2（ox）（p-PhDTA）2（H2O）10]·6H2O （ox = oxalate）, which was characterized by single-crystal X-ray diffraction （MoKα radiation, = 0.71073）, elemental analysis and IR. This complex crystallizes in the monoclinic system, space group P21/n with a = 10.2522（8）, b = 10.0053（8）, c = 23.8834（18）, = 99.1080（10）°, V = 2419.0（3）3, Z = 2, Mr = 1367.32, Dc = 1.877 g/cm3, F（000） = 1368, = 2.830 mm-1, the final R = 0.0337 and wR = 0.0794 for 4747 observed reflections （I 〉 2 （I））. The exo-tetradentate oxalate ligand, generated in situ from the oxidative coupling of methanol, is incorporated to construct a dinuclear Gd2（ox）2 unit decorated with p-PhDTA ligands on the two sides with a monodentate coordination mode. The dinuclear molecules are further connected by the lattice water molecules to form a three-dimen- sional hydrogen network.

关 键 词：Gd（III） complex crystal structure p-phenylenediamine-N N N＇ N＇-tetraaceticacid OXALATE 

分 类 号：O627.8[理学—有机化学]