Synthesis, Characterization, and Structure of [GaCl3(NHC)] Complexes

The reaction of GaCl3 with 1 equiv of NHC ligand (NHC = N-heterocyclic carbene) at room temperature in pentane yielding the corresponding 1:1 adduct [GaCl3(NHC)] is reported. Using IPr (N,N‘-bis(2,6-diisopropylphenyl)imidazol-2-ylidene), IMes (N,N‘-bis(2,4,6-trimethylphenyl)imidazol-2-ylidene), and IPrMe (1,3-diisopropyl-4,5-dimethylimidazol-2-ylidene), three NHC-containing GaIII adducts have been synthesized in good yields and fully characterized by 1H and 13C NMR, HRMS, elemental analysis, and X-ray diffraction studies for the first time. The solid-state structure of [GaCl3(IMes)] presented, as a special feature, two different positions of the main molecule with an occupation ratio of 50%. These positions of the molecule are shifted with respect to each other along the c-axis by 0.96 Å.本文报道了三氯化镓（GaCl₃）与1当量氮杂环卡宾（N-heterocyclic carbene，缩写NHC）配体在室温下于戊烷溶剂中反应，生成对应1:1加合物[GaCl₃(NHC)]的合成过程。采用IPr（N,N'-双(2,6-二异丙基苯基)咪唑-2-卡宾）、IMes（N,N'-双(2,4,6-三甲基苯基)咪唑-2-卡宾）及IPrMe（1,3-二异丙基-4,5-二甲基咪唑-2-卡宾）三种配体，首次以良好收率合成了三种含NHC的三价镓加合物，并通过1H核磁共振谱、13C核磁共振谱、高分辨质谱（HRMS）、元素分析及X射线衍射分析对其进行了全面表征。本文所报道的[GaCl₃(IMes)]固态结构具有特殊结构特征：主分子存在两种空间排布，二者占有率均为50%；两种排布沿晶胞c轴方向相互偏移0.96埃（Å）。