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Facile and rapid synthesis of crystalline quadruply bonded Cr(ii) acetate coordinated with axial ligands

机译：与轴配体协调的乙酸晶四（II）的晶体高键合Cr（II）的舒适性和快速合成

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A quadruple bond formed between d-block or f-block atoms is an interesting research topic due to its unique nature including a supershort bonding distance and narrow energy gap between delta and delta*. Among various multiply bonded complexes, quadruply bonded Cr(ii) acetates are considered useful to control the delta-delta* energy gap by the Lewis basicity of additional ligands. However, the synthesis and preparation of the high-quality, large-sized crystals of Cr(ii) acetates coordinated with axial ligands (Cr-2(OAc)(4)L-2) have been difficult due to their vulnerability to O-2, a representative oxidizing agent under aerobic conditions. In this study, we report a facile synthesis of sub-millimeter-scale crystals of Cr-2(OAc)(4)L-2 by simple dissolution of Cr-2(OAc)(4) in ligand solvents L. To obtain stably ligated Cr-2(OAc)(4)L-2, anhydrous Cr(ii) acetates (Cr-2(OAc)(4)) were dissolved in the ligand solvents L, which was degassed of dissolved O-2. Also, sub-millimeter-scale single crystals of Cr-2(OAc)(4)L-2 were produced rapidly for less than an hour by the drop-drying process. The single-crystalline phase of the synthesized Cr(ii) complexes was measured by X-ray diffraction techniques, confirming the dependency of Lewis basicity of the additional axial ligands on the Cr-Cr quadruple bond distance. Further, the Raman peaks of the quadruple bonds in Cr-2(OAc)(4)L-2 were observed to be red-shifted with the increased basicity of the axial ligands.
机译：由于其独特的性质，在D-Block或F块原子之间形成的四重粘结是一种有趣的研究课题，包括超箭粘接距离和Delta和Delta *之间的窄能隙。在各种繁殖粘合的络合物中，二次键合的Cr（II）乙酸盐被认为是可用于通过另外配体的lewis碱度控制Δ-delta *能量差距。然而，由于其对O-易受伤害而协调的Cr（II）Cr（II）乙酸盐的合成和制备乙酸盐（CR-2（OAC）（4）L-2）的含量较难2，在有氧条件下代表性氧化剂。在该研究中，通过简单地溶解配体溶剂L中的Cr-2（OAC）（4）的简单溶解来报告Cr-2（4）（4）L-2的亚毫米级晶体的容易合成。将连接的Cr-2（OAC）（4）L-2，无水Cr（II）乙酸盐（Cr-2（OAc）（4））溶解在配体溶剂L中，溶解O-2脱气。此外，通过滴剂过程快速生产Cr-2（OAC）（4）（4）L-2的亚毫米级单晶，少于一个小时。通过X射线衍射技术测量合成的Cr（II）配合物的单晶相，证实了Lewis碱度对CR-CR四重键距离的依赖性轴向配体的依赖性。此外，将观察到Cr-2（OAC）（4）L-2中的四重键的拉曼峰，以随着轴向配体的碱度增加而被红移。

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    《RSC Advances》 |2019年第42期|共6页
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