3个零维自由基-过渡金属配合物的合成及结构表征

在常温溶剂挥发法的条件下,利用NITpPy (2-(4-吡啶基)-4,4,5,5-四甲基-4,5-二氢-1H-咪唑-3-氧化物)和对硝基苯甲酸(Hpnba)与过渡金属离子组装,得到了3个单核零维结构、未见报道的金属-自由基配合物M(pnba)2(NITpPy)2] {M=Co (1),Cd (2),Zn (3)}.X射线单晶衍射结果表明3个配合物为同晶结构,都为中心对称的单斜晶系C2/c空间群 (No.15).3个配合物的金属离子都位于对称反演中心,具有变形的四面体构型,分别被2个NITpPy的吡啶N原子和2个pnba-的羧基O原子占据.TGA测试表明它们都具有较好的热稳定性.另外,使用X射线粉末衍射、红外光谱、元素分析对其进行光谱表征.

Synthesis and characterization of three discrete radicals-transitionmetal complexes with nitronyl nitroxide

Three new discrete metal-radical complexes, namely, M(pnba)2(NITpPy)2]{M=Co(1), Cd(2), Zn(3)} were synthesized under solvent evaporation conditions at room temperature via the self assembly of NITpPy=2-(4-pyridyl)-4, 4, 5, 5-tetramethyl-4, 5-dihydro-1H-imidazolyl-1-oxyl-3-oxide and Hpnba=p-nitrobenzoic acid with transition metals.Single-crystal X-ray diffraction analysis reveals that complexes 1, 2 and 3 are isomorphous and crystallized in the monoclinic space group C2/c(No.15).The three complexes are centrosymmetrical with the metal atoms in the inversion center and in disordered tetrahedral geometry coordinated by two radical ligands of nitrogen atoms and two pnba oxygen atoms.Further characterizations of the three complexes, including thermal analysis, powder X-ray diffraction, infrared spectroscopy, and elemental analysis were also performed.