Synthesis and Crystal Structure of Dicopper(II) Compound Containing Oxalate and Reduced Imino Nitrox

• 作 者: 李立存 董朝灵 廖代正 姜宗慧 阎世平
• 机 构: Department of Chemistry, State Key Laboratory of Structural Chemistry
• 出 处: 结构化学
• 发表日期: 2004年期
• 关键词: crystal structure reduced nitroxide radical dicopper compound oxagte bridge

A new dicopper(II) compound with oxalate and reduced imino nitroxide radicals [Cu2(t-C2O4)(Him2-py)2(H2O)2] (NO3)2 (Him2-py= 1-hydroxy-2-(2'-pyridyl)-4,4,5,5-tetramethylimidazoline) has been synthesized and its crystal structure was determined by X-ray diffraction method. The complex crystallizes in monoclinic, space group P21/n with a=9.913(4), b =19.057(8), c=10.169(4) A, β=114.292(7)°, V=1751 (1) A3, C26H38Cu2N8O 14, Mr=813.72, Dc =1.543 g/cm3,μ(MoKa)=1.290 mm-1, F(000)=840, Z=2, the final R=0.0398 and wR=0.0986for 1878 observed reflections (I＞2σ(I)). The imino nitroxide 2-(2'-pyridyl)-4,4,5,5-tetramethylimidazoline-l-oxyl (im2-py) is reduced in the reaction to yield Him2-py which consists of oxalato-bridged centrosymmetric [Cu2(μ-C2O4)(Him2-py)2(H2O)2]2+ ions and noncoordinnted NO3- anions. Each copper(II) ion is in a distorted tetragonal pyramid environment: two niuogen atoms from Him2-py and two oxygen atoms from the oxalate group are in the basal plane, and one water molecule at the axial position.