高等学校化学学报

高等学校化学学报 ›› 2013, Vol. 34 ›› Issue (3): 520.doi: 10.7503/cjcu20120733

• 研究论文: 无机化学 • 上一篇    下一篇

铬酸根桥联Cu(Ⅱ)/Ni(Ⅱ)链状配位聚合物的合成及性质

蔡良圆1, 齐琪2, 杨春3, 江山1, 姜谦1, 王庆伦1, 任红霞2   

  1. 1. 南开大学化学系, 天津 300071;
    2. 南开大学先进能源材料化学教育部重点实验室, 天津 300071;
    3. 河北工业大学化工学院, 天津 300130
  • 收稿日期:2012-08-10 出版日期:2013-03-10 发布日期:2013-02-18
  • 通讯作者: 王庆伦,男,博士,副教授,主要从事功能配合物和分子磁学研究.E-mail:wangql@nankai.edu.cn;任红霞,女,博士,讲师,主要从事配位聚合物的研究.E-mail:csxh3605@sina.com.cn E-mail:wangql@nankai.edu.cn;csxh3605@sina.com.cn
  • 基金资助:

    国家自然科学基金(批准号:21071085,21101096,90922032)、天津市自然科学基金(批准号:11JCYBJC03500)和河北省自然科学基金(批准号:B2012202106)资助.

Synthesis and Characterization of Chromate Cu(Ⅱ)/Ni(Ⅱ) Chain Complexes

CAI Liang-Yuan1, QI Qi2, YANG Chun3, JIANG Shan1, JIANG Qian1, WANG Qing-Lun1, REN Hong-Xia2   

  1. 1. Department of Chemistry, Nankai University, Tianjin 300071, China;
    2. Key Laboratory of Advanced Energy Materials Chemistry, Ministry of Education, Nankai University, Tianjin 300071, China;
    3. School of Chemical Engineering and Technology, Hebei University of Technology, Tianjin 300130, China
  • Received:2012-08-10 Online:2013-03-10 Published:2013-02-18

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被引次数

2

摘要：

设计合成了2个一维链状铬酸根桥连的配位聚合物(NH4)2[Cu(NH3)2(CrO4)2](1)和(NH4)2·[Ni(NH3)2(CrO4)2](2), 并对其进行了X射线单晶结构分析、 热重-差热分析和多种磁学测试. 晶体结构分析表明, 2个配合物的晶体均属于三斜晶系, 空间群均为P1. 配合物1的晶胞参数为: a=0.59090(12)nm, b=0.6929(3) nm, c=0.73740(15) nm, α=107.03(4)°, β=92.79(3)°, γ=112.44(2)°; 配合物2的晶胞参数为: a=0.56987(7)nm, b=0.69972(9) nm, c=0.73335(8)nm, α=104.929(3)°, β=96.121(3)°, γ=112.325(4)°. 热重分析结果表明, 配合物1和2均在150 ℃左右开始分解, 生成H2Cr2CuO5和H2Cr2NiO5, 在410 ℃以上继续分解, 脱水得到相应的氧化物. 配合物的变温磁化率测试结果表明, 相邻Cu(Ⅱ)离子(配合物1)或Ni(Ⅱ)离子(配合物2)之间存在较弱的反铁磁相互作用; 低温变场和交流磁化率测试结果表明, 2个配合物均为反铁磁体.

关键词: 一维结构, 配位聚合物, 晶体结构, 热分析, 磁性表征

Abstract:

Two new one-dimensional chain complexes, (NH4)2[Cu(NH3)2(CrO4)2](1) and (NH4)2·[Ni(NH3)2(CrO4)2](2), were obtained by mixing copper nitrate or nickel nitrate with the same molar of ammonium dichromate in ammonia water at room temperature, and they were characterized by single-crystal X-ray diffraction(XRD), thermogravimetric analysis(TGA) and differential thermal analysis(DTA). Furthermore, the complexes were magnetically characterized by temperature-dependent magnetic susceptibility, field-dependent magnetization, and alternate current(AC) magnetic measurements. The structure analysis results show that crystals of both complexes are triclinic, space group P1 with a=0.59090(12) nm, b=0.6929(3) nm, c=0.73740(15) nm, α=107.03(4)°, β=92.79(3)°, γ=112.44(2)° for Cu(Ⅱ) complex and a=0.56987(7) nm, b=0.69972(9) nm, c=0.73335(8) nm, α=104.929(3)°, β=96.7121(3)°, γ=112.325(4)° for Ni(Ⅱ) complex. In the crystal structure, the [M(NH3)2]2+ units are linked by two chromato bridges, forming an eight-member ring. As a whole, both complexes have one-dimensional chain structures. The two complexes began to break down as the temperature gradually reached 150 ℃ or so, leaving behind H2Cr2CuO5 and H2Cr2NiO5, and afterwards they are dehydrated at above 410 ℃. The temperature-dependent magnetic susceptibilities were measured in the range of 2—300 K, which implies a weak antiferromagnetic interaction between the adjacent mental ions. The field-dependent magnetization and AC magnetic measurements indicate that the two complexes are both antiferromagnets.

Key words: One-dimensional(1D) structure, Coordination polymer, Crystal structure, Thermal analysis, Magnetic characterization

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