高等学校化学学报

高等学校化学学报 ›› 1993, Vol. 14 ›› Issue (6): 745.

• 研究论文 • 上一篇    下一篇

四苯基[b,f,j,n][1,5,9,13]四氮杂环十六碳炔镍轴向氮碱加合物的合成、结构和性质研究

李明星1, 徐正1, 李金玉1, 游效曾1, 王化勤1, 杨跃1, 俞运鹏2, 朱多林2   

  1. 1. 南京大学配位化学研究所, 配位化学国家重点实验室, 材料分析中心, 南京 210008;
    2. 镇江师范专科学校
  • 收稿日期:1992-10-05 修回日期:1992-11-29 出版日期:1993-06-24 发布日期:1993-06-24
  • 通讯作者: 徐正.
  • 基金资助:

    国家科委基础性研究重大课题;国家自然科学基金

Synthesis, Crystal Structure and Properties of TAAB Nickel Adducts with Axial N-Base Ligands

LI Ming-Xing1, XU Zheng1, LI Jin-Yu1, YOU Xiao-Zeng1, WANG Hua-Qin1, YANG Yue1, YU Yun-Peng2, ZHU Duo-Lin2   

  1. 1. Coordination Chemistry Institute, Coordination Chemistry State Key Laboratory, Center for Materials Analysis, Nanjing University, Nanjing, 210008;
    2. Department of Chemistry, Zhenjiang Normal College, Zhenjiang, 212003
  • Received:1992-10-05 Revised:1992-11-29 Online:1993-06-24 Published:1993-06-24

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摘要： 合成了3个四苯基[b,f,j,n][1,5,9,13]四氮杂环十六碳炔镍轴向氮碱加合物[Ni(TAAB)(L)2](BF4)2(L为吡啶、咪唑、DMF)以及4,4'-联吡啶桥联配合物[Ni(TAAB)(μ-4,4'-bipy)]。[(ClO4)2·H2O]。用元素分析、IR和热分析对标题化合物作了表征。双吡啶加合物的晶体结构显示,TAAB大环呈马鞍形结构,轴向配位的吡啶环平面相互垂直,轴向的2个Ni—N键长明显比赤道平面的4个Ni—N键长大,形成拉长的配位八面体。4,4'-联吡啶配合物的变温磁化率表明,镍(Ⅱ)离子间存在反铁磁性磁交换相互作用。

关键词: 轴向配位, TAAB大环, 镍配合物, 晶体结构, 磁交换作用

Abstract: Four adducts of Py, Im, DMFand 4,4'-bipy with Ni(TAAB)2+, where TAAB=tetraben-zo[b,f,j,R][1,5,9,13]tetraazacyclohexadecine, were synthesized and characterized by elementary analysis, IRand thermal analysis.The crystal structure of [Ni(TAAB)(Py)2](BF4)2has been determined.The crystal belongs to a monoclinic system with space group P21/n, α=1.6465(6) nm, b=1.2486(5) nm, c=2.0219(1) nm,β=113.79°, V=3.8039 nm3, Z=4, R=0.068.TAABmacrocyclic ligand presents a decidedly saddle-shaped appearance.The planes of two pyridine molecules are perpendicular to each other.The bond distances of Ni-N(n)(n=10,20,30,40) are in the range of 0.1983-0.2043 nm while the bond distances of Ni-N(B)(n=5,6) are 0.2182-0.2189 nm, forming a distorted octahedron coordination geometry around nickel ion.The variable-temperature magnetic susceptibility of 4,4'-bipyridine-bridging nickel TAABcomplex obeys the Curi-er-Weiss law (θ=- 44 K) and indicates an antiferromagnetic exchange interaction between nickel ions.

Key words: Axial coordination, TAAB macrocyclic, Nickel complex, Crystal structure, Magnetic exchange interaction

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