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Exploring the Limits of Ligand Rigidification in Transition Metal Complexes with Mono-N-Functionalized Pyclen Derivatives
Inorganic Chemistry ( IF 4.3 ) Pub Date : 2024-02-13 , DOI: 10.1021/acs.inorgchem.3c04451 Gwladys Nizou 1 , Zoltán Garda 2 , Enikő Molnár 2 , David Esteban-Gómez 3 , Mariane Le Fur 1 , Olivier Fougère 4 , Olivier Rousseaux 4 , Carlos Platas-Iglesias 3 , Raphaël Tripier 1 , Gyula Tircsó 2 , Maryline Beyler 1
Inorganic Chemistry ( IF 4.3 ) Pub Date : 2024-02-13 , DOI: 10.1021/acs.inorgchem.3c04451 Gwladys Nizou 1 , Zoltán Garda 2 , Enikő Molnár 2 , David Esteban-Gómez 3 , Mariane Le Fur 1 , Olivier Fougère 4 , Olivier Rousseaux 4 , Carlos Platas-Iglesias 3 , Raphaël Tripier 1 , Gyula Tircsó 2 , Maryline Beyler 1
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We report the synthesis of a new family of side-bridged pyclen ligands. The incorporation of an ethylene bridge between two adjacent nitrogen atoms was reached from the pyclen-oxalate precursor described previously. Three new side-bridged pyclen macrocycles, Hsb-3-pc1a, sb-3-pc1py, and Hsb-3-pc1pa, were obtained with the aim to assess their coordination properties toward Cu2+ and Zn2+ ions. We also prepared their nonreinforced analogues H3-pc1a, 3-pc1py, and H3-pc1pa as comparative benchmarks. The two series of ligands were characterized and their coordination properties were investigated in detail. The Zn2+ and Cu2+ complexes with the nonside-bridged series H3-pc1a, 3-pc1py, and H3-pc1pa were successfully isolated and their structures were assessed by X-ray diffraction studies. In the case of the side-bridged family, the synthesis of the complexes was far more difficult and, in some cases, unsuccessful. The results of our studies demonstrate that this difficulty is related to the extreme stiffening and basicity of such side-bridged pyclens.
中文翻译：
使用单 N 官能化 Pyclen 衍生物探索过渡金属配合物中配体刚性化的极限
我们报告了新的侧桥 Pyclen 配体家族的合成。两个相邻氮原子之间乙烯桥的结合是从先前描述的pyclen-草酸酯前体实现的。获得了三种新的侧桥pyclen大环化合物H sb-3-pc1a 、 sb-3-pc1py和H sb-3-pc1pa ，目的是评估它们对Cu 2+和Zn 2+离子的配位特性。我们还准备了他们的非增强类似物 H 3-pc1a 、 3-pc1py和 H 3-pc1pa作为比较基准。对这两个系列的配体进行了表征，并详细研究了它们的配位特性。成功分离出具有非侧桥系列 H 3-pc1a 、 3-pc1py和 H 3-pc1pa的 Zn 2+和 Cu 2+配合物，并通过 X 射线衍射研究评估了它们的结构。对于侧桥家族，复合物的合成要困难得多，在某些情况下甚至不成功。我们的研究结果表明，这种困难与这种侧桥pyclens的极端硬化和碱性有关。
更新日期：2024-02-13
中文翻译：
使用单 N 官能化 Pyclen 衍生物探索过渡金属配合物中配体刚性化的极限
我们报告了新的侧桥 Pyclen 配体家族的合成。两个相邻氮原子之间乙烯桥的结合是从先前描述的pyclen-草酸酯前体实现的。获得了三种新的侧桥pyclen大环化合物H sb-3-pc1a 、 sb-3-pc1py和H sb-3-pc1pa ，目的是评估它们对Cu 2+和Zn 2+离子的配位特性。我们还准备了他们的非增强类似物 H 3-pc1a 、 3-pc1py和 H 3-pc1pa作为比较基准。对这两个系列的配体进行了表征，并详细研究了它们的配位特性。成功分离出具有非侧桥系列 H 3-pc1a 、 3-pc1py和 H 3-pc1pa的 Zn 2+和 Cu 2+配合物，并通过 X 射线衍射研究评估了它们的结构。对于侧桥家族，复合物的合成要困难得多，在某些情况下甚至不成功。我们的研究结果表明，这种困难与这种侧桥pyclens的极端硬化和碱性有关。
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