| 基于烟酰腙Schiff碱的Cu(Ⅱ)和Ni(Ⅱ)配合物的合成、晶体结构和性质 |
| Syntheses, Crystal Structures and Properties of Copper(Ⅱ) and Nickel(Ⅱ) Complexes Based on Nicotinoyl Hydrazone Schiff Base |
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| 摘要: 采用缓慢挥发法合成了2个烟酰腙类Schiff碱配合物[Cu(Py)(HL1)]2 (1)和[Ni(L2)2] (2), 其中, H3L1=2, 4-二羟基苯甲醛缩烟酰腙, HL2=2-乙酰基吡啶缩烟酰腙。采用元素分析、红外光谱、紫外光谱、荧光光谱和热重分析以及X-射线单晶衍射分析进行了表征。结果表明, 1和2的晶体均属单斜晶系, P21/c空间群;1的晶胞参数a=0.739 86(12) nm, b=1.903 7(3) nm, c=1.154 86(19) nm, β=105.090(3)°, V=1.570 5(4) nm3;该化合物是中心对称的双核配合物, 每个Cu(Ⅱ)离子都处于畸变四方锥配位环境;结构基 元通过π-π相互作用和O-H…N氢键形成三维超分子。2的晶胞参数a=2.034 0(5) nm, b=1.183 2(3) nm, c=1.020 7(3) nm, V=2.456 1(11) nm3;中心离子Ni(Ⅱ)的配位数为6, 它处于畸变八面体配位环境。配合物有很高的热稳定性, 分解温度分别为315 ℃ (1)和358 ℃ (2)。 |
| 关键词: 烟酰腙 配合物 晶体结构 热稳定性 |
| 基金项目: 福建省教育厅A类重点项目(No.JA14261), 2014年国家级大学生创新创业训练计划项目(No.201410399017)资助。 |
| Abstract: The copper(Ⅱ) and nickel(Ⅱ) complexes of nicotinoyl hydrazone Schiff base, [Cu(Py)(HL1)]2 (1) and [Ni(L2)2] (2), where H3L1 is pyridine-3-carboxylic acid (2,4-dihydroxy-benzylidene)hydrazide, HL2 is pyridine-3-carboxylic acid (pyridine-2-yl ethylidyne)hydrazide, were respectively synthesized by slow evaporation methods in mixed-solvent, and characterized by elemental analysis, IR, UV-Vis, FL spectra, TGA and single crystal X-ray diffraction. The crystals of 1 and 2 belongs to the monoclinic system, space group P21/c with cell parameters (1) a=0.739 86(12) nm, b=1.903 7(3) nm, c=1.154 86(19) nm, β=105.090(3)°, V=1.570 5(4) nm3 and (2) a=2.034 0(5) nm, b=1.183 2(3) nm, c=1.020 7(3) nm, V=2.456 1(11) nm3. The complex 1 is a centrosymmetric binuclear complex with Cu(Ⅱ) ions in square pyramidal geometry. The structure units of 1 are linked by intermolecular π-π interactions and O-H…N hydrogen bonds, forming three-dimensional supermolecular network. In 2, the Ni(Ⅱ) ions act as distorted octahedral geometry, being surrounded by two imine nitrogen atoms, two deprotonated amide oxygen atoms and two pyridyl nitrogen atoms from two monovalence anions of HL2 ligand. The tests showed the two complexes displayed good thermal stability below 315 ℃ (1)和358 ℃ (2), respectively. |
| Keywords: nicotinoyl hydrazone complexes crystal structure thermal stability |
| 投稿时间：2015-04-11 修订日期：2015-05-27 |
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| 储召华,解庆范,李颖茜,陈延民.基于烟酰腙Schiff碱的Cu(Ⅱ)和Ni(Ⅱ)配合物的合成、晶体结构和性质[J].无机化学学报,2015,31(7):1380-1386. |
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