首页> 外文期刊>Journal of chemical crystallography >Synthesis, crystal structure and electrochemical property of new rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene) bis(azido)cobalt(III) nitrate methanol solvate complex
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Synthesis, crystal structure and electrochemical property of new rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene) bis(azido)cobalt(III) nitrate methanol solvate complex

机译:新型rac-5,5,7,12,12,14-六甲基-1,4,8,11-四氮杂环十四烷-4,11-二烯)硝酸双(叠氮基)钴(III)的合成,晶体结构和电化学性质甲醇溶剂合物

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摘要

The new cobalt compound, [Co(C_(16)H_(35)N _(10)]~+(NO_3)~-?CH_3OH (1), have been synthesized and characterized. It's structure and electrochemical property were investigated using single-crystal X-ray diffraction and cyclic voltammetry in solutions of dimethyl sulfoxide (DMSO) and methanol (CH _3OH). The X-ray diffraction analysis reveals that 1 crystallizes in the monoclinic space group P2_1/c with a = 9.8339 (10) ?, b = 16.4048 (17) ?, c = 15.3628 (16) ?, β = 104.96 (9)° and Z = 4. The complex 1 consists of one [Co(C_(16)H_(35)N _(10))]~+ cation, one NO_3~- anions and one solvent CH_3OH molecule. The metal center of complex 1 is six-coordinated, with the four nitrogens of the macrocycle defining an equatorial plane and two axially ligated [N_3]~- ions completing the cobalt coordination sphere. Moreover, hydrogen bonds of O-H?N, O-H?O and N-H?O and static force connect two components of the compound and maintain the crystal structure. Additionally, in situ spectro-electrochemical measurements support Co(III)/Co(II) reversible reduction processes with the observation of the corresponding spectral changes with the applied potentials E _(app) = -1.5 and 0.5 V. The results obtained by the method are in agreement with those by the CV methods.
机译:合成了新型钴化合物[Co(C_(16)H_(35)N _(10)]〜+(NO_3)〜-?CH_3OH(1),并对其结构和电化学性能进行了研究。二甲基亚砜(DMSO)和甲醇(CH _3OH)溶液中的结晶X射线衍射和循环伏安法X射线衍射分析表明,在单斜空间群P2_1 / c中有1个晶体,a = 9.8339(10)? ,b = 16.4048(17)?,c = 15.3628(16)?,β= 104.96(9)°,Z =4。配合物1由一个[Co(C_(16)H_(35)N _(10 ))]〜+阳离子,一个NO_3〜-阴离子和一个溶剂CH_3OH分子。配合物1的金属中心是六配位的,大环的四个氮原子定义一个赤道面,两个轴向连接的[N_3]〜-离子此外,OH?N,OH?O和NH?O的氢键以及静力将化合物的两个成分连接起来并保持晶体结构。保证支持Co(III)/ Co(II)可逆还原过程,并观察到相应的光谱变化,其中施加电势E _(app)= -1.5和0.5V。该方法获得的结果与通过简历方法。

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