Synthesis, structural and spectroscopic characterization of the bis(nitrito-<i>N</i>) octaethylporphyrin cobalt(III) complex

• 作者: Bader Belhaj Ali Habib Nasri Michel Giorgi Mohamed Salah Belkhiria
• 来源期刊: 无机化学期刊(英文)
• 学科: 化学
• 关键词: Cobalt(III) PORPHYRIN X-Rays Diffraction UV-VISIBLE 1H NMR
• 年，卷（期）: 2011,（3）
• 页码范围: 39-46
• 页数: 8页
• 分类号: O6

摘要

The bis(nitrito-N) cobalt(III) octaethylporphyrin derivative with the formula [K(18-C-6)(NO2)0.5(H2O)0.5]2 [CoIII(OEP)(NO2)2] (1) (OEP = octaethylporphyrin and 18-C-6 is the crown ether18-crown-6) has been synthesized and characterized by UV-vis, IR and proton NMR spectroscopy which indicate, inter alia, that the cobalt ion presents the oxidation state III. The synthesis utilizes 18-crown-6 to solubilize potassium nitrite in the synthetic procedure. This compound crystallizes in the triclinic system, with the centric space group P-1 and the following unit cell parameters: 11.6724(2) ?, b = 12.5715(2) ?, c = 13.4722(3) ?, α = 101.1290(6)°, β = 106.6498(6)°, γ= 109.1507(6)°, Z = 1 and V = 1696.74(5) ?3. The crystal structure has been solved and refined to R = 0.0499 and R(w) = 0.1319. The X-rays molecular structure of 1 shows that there is a relatively close interaction of both two NO2- axial ligands of the ion complex [CoIII(OEP)(NO2)2]- with the potassium atoms of the two counterions [K(18-C-6) (NO2)0.5(H2O)0.5]0.5+. The title compound exhibits one-dimension polymer-like structure where “monomers” are linked together through strong O(H2O)—H…O(nitrito-O) hydrogen bonds.