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化学学报
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化学学报 ›› 1997, Vol. 55 ›› Issue (9): 892-900. 上一篇    下一篇

研究论文

含四氮杂十四元大环配体过渡金属配正离子与双(N-氰基亚胺基二硫甲酸)合镍负离子加合物的合成、表征和[Ni(hmtade)][Ni(cdc)2]的晶体结构

李金山;谢斌   

  1. 南开大学元素有机化学研究所;四川轻化工学院基础部
  • 发布日期:1997-09-15

Synthesis and characterization of adducts of transition-metal complex cations containing tetra-azatetradeca-membered ring ligands with bis (N-cyanodithiocarbimato) nickelate anion and crystal structure of [Ni(hmtade)][Ni(cdc)2]

LI JINSHAN;XIE BIN   

  • Published:1997-09-15

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合成了七个含四氮杂十四元大环配体过渡金属配正离子与双(N-氰基亚胺基二硫代甲酸)合镍负离子的加合物[ML][Ni(cdc)2](cdc=N-氰基亚胺基二硫代甲酸根; L=hmtade,hmta, dmtade, tmtate; M=Cu, Ni, Zn), 通过元素分析、红外光谱、电子光谱、磁化率和顺磁共振谱对加合物结构进行了表征。测定了[Ni(hmtade)][Ni(cdc)2]的晶体结构, 其晶体属单斜晶系, C2/c空间群, 晶胞参数: a=1.1883(2), b=1.1753(2),c=2.0482(4)nm, α=90°, β=100.19(1)°, γ=90°,V=2.8154nm^3, Mr=630.19, Dx=1.482g/cm^3, Z=4, 对正负离子间的相互作用进行了讨论。

关键词: 红外分光光度法, 元素分析, 晶体结构, 氮杂环化合物, 顺磁共振, 镍络合物, 硫代甲酸 P

Seven adducts of transition-metal complex cations containing tetra-azatetradeca-membered ring ligands with bis (N-cyanodithiocarbimato) nickelate anion, [ML][Ni(cdc)2] (cdc=N-cyanodithiocarbimate; L=hmtade, hmta, dmtade, tmtate; M=Cu, Ni, Zn), have been synthesized. The structures of these adducts have been characterized by elemental analysis, infrared spectra, electronic spectra, electron paramagnetic resonance spectra and magnetic susceptibility. The crystal structure of [Ni(hmtade)][Ni(cdc)2] has been determined. The crystal belongs to monoclinic, space group C2/c. The cell parameters are a=1.1883(2), b=1.1753(2), c=2.0482(4)nm, α=90°, β=100.19(1)°, γ=90°, V=2.8154nm^3, Mr=630.19, Dx=1.482g/cm^3, Z=4. The interaction between cation and anion has been discussed.

Key words: INFRARED SPECTROPHOTOMETRY, ELEMENTAL ANALYSIS, CRYSTAL STRUCTURE, NITROGEN HETEROCYCLICS, PARAMAGNETIC RESONANCE, NICKEL COMPLEX, METHANETHIOIC ACID P

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