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首页> 外文期刊>Journal of thermal analysis and calorimetry >Transition Metal Complexes with Pyrazole Based Ligands part 15. Cobalt(III)-, nickel(II)- and copper(II)-complexes with 3,5-dimethyl-1-thiocarboxamidepyrazole
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Transition Metal Complexes with Pyrazole Based Ligands part 15. Cobalt(III)-, nickel(II)- and copper(II)-complexes with 3,5-dimethyl-1-thiocarboxamidepyrazole

机译:带有吡唑基配体的过渡金属配合物,第15部分。钴(III)-,镍(II)-和铜(II)-配合物与3,5-二甲基-1-硫代羧酰胺吡唑的配合

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摘要

The complex formation of cobalt(II)-, nickel(II) and copper(II) sulphate hydrates with 3,5-dimethyl-1-thiocarboxamidepyrazole (HL) was studied. The influence of the anions on the course of the reaction was also examined, using nickel(II) salts with various anions. Beside the NiSO_4·7H_2O the reaction has been carried out with Ni(OAc)_2, Ni(CF_3COO)_2 and Ni(SCN)_2. Compounds with the following composition were obtained: Co(L)_3, Ni(L)_2 and [Cu(SCN)L]_2. The structure of the ligand and the Co(L)_3 complex was determined by single crystal X-ray analysis, while that of the Ni(L)_2 was solved by analysis of powder diffraction X-ray data. The most probable structure of the copper(II) complex is proposed on the basis of the elemental analyses data, FT-IR spectrometry and magnetic measurement. The thermal decomposition of the complexes was investigated by thermogravimetry, DSC and coupled TG-MS measurements. In the case of the nickel(II) compound, a relatively stable intermediate was detected in the 550-650 K temperature range. The composition of the intermediate, Ni(SCN)(NCS), was determined by FT-IR-spectrometry.
机译:研究了钴(II​​)-,镍(II)和铜(II)与3,5-二甲基-1-硫代羧酰胺吡唑(HL)的络合物形成。还使用带有各种阴离子的镍(II)盐检查了阴离子对反应过程的影响。除NiSO_4·7H_2O以外,反应还与Ni(OAc)_2,Ni(CF_3COO)_2和Ni(SCN)_2进行。获得具有以下组成的化合物:Co(L)_3,Ni(L)_2和[Cu(SCN)L] _2。通过单晶X射线分析确定了配体和Co(L)_3配合物的结构,而通过粉末衍射X射线数据分析了Ni(L)_2的结构。根据元素分析数据,FT-IR光谱和磁测量,提出了铜(II)配合物最可能的结构。配合物的热分解通过热重分析,DSC和耦合TG-MS测量进行了研究。对于镍(II)化合物,在550-650 K的温度范围内检测到相对稳定的中间体。通过FT-IR光谱法确定中间体Ni(SCN)(NCS)的组成。

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