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合成并表征了质子化的 N - (二茂钌基甲基 ) - 1,4 ,7-三氮杂 - 9-冠 - 3(1)和 N ,N′,N″-三 - (二茂钌基甲基 ) - 1,4 ,7-三氮杂 - 9-冠 - 3(2 ) .用 X射线衍射法测定了化合物 2的结构 .化合物 2的晶体属 P2 1/ a空间群 .晶胞参数 a=1.4 2 85(3) nm,b=1.9888(3) nm,c=1.9133(3) nm;β=10 9.12 (2 )°;V=5.1358(1.0 ) nm3 ;Z=4 .Dc=1.6 6 5g/ cm3 . 1和 2的核磁共振谱表明 ,化合物中取代 Cp环上质子的共振吸收较二茂钌 Cp环上质子的吸收向低场移动 .这表明质子化的 1,4 ,7-三氮杂 - 9冠 - 3对 Cp环上质子具有去屏蔽作用 .化合物 2的电位扫描曲线在 0 .84 V处出现一个氧化波
The synthesis and characterization of protonated N - (lrromanylmethyl) -1,4,7-triaza-9-crown-3 (1) and N, N ’, N " Rutheniummethyl) -1,4,7-triaza-9-crown-3 (2). The structure of compound 2 was determined by X-ray diffraction.The crystal of compound 2 belongs to the P2 1 / a space group. Cell parameters a = 1.4 2 85 (3) nm, b = 1.9888 (3) nm, c = 1.9133 (3) nm; β = 10 9.12 (2) °; V = 5.1358 = 1.6 6 5 g / cm3 The NMR spectra of 1 and 2 show that the resonance absorption of the protons replacing the Cp ring in the compound shifts lower than that of the proton on the ring of the ruthenocene Cp. This shows that the protonated 1,4, The 7-triaza-9-crown-3 has a deprotection effect on the proton on the Cp ring. The potential sweep curve of compound 2 shows an oxidation wave at 0.84 V