Hydrothermal synthesis of Group 13 metal trifluoride complexes with neutral N-donor ligands
作者:Rajiv Bhalla、William Levason、Sajinder K. Luthra、Graeme McRobbie、Francesco M. Monzittu、Jazmyn Palmer、Gillian Reid、George Sanderson、Wenjian Zhang
DOI:10.1039/c5dt01120e
日期:——
[K(2,2,2-crypt)]F. Crystallisation of a mixture of [NH4][PF6] and [GaF3(terpy)]·3H2O from aqueous solution produced the edge-bridged cationic complex, [Ga(terpy)F}2(μ-F)2][PF6]2. The synthesis of the more sterically bulky [GaCl3(tBu3-terpy)] (tBu3-terpy = 4,4′4′′-tris-tBu-2,2′:6′,2′′-terpyridyl) and the crystal structure of [GaCl2(tBu3-terpy)][GaCl4], which contains a trigonal bipyramidal cation, are
水合的13族氟化物,MF 3 ·3H 2 O(M = Al,Ga或In)与2,2':6',2''-吡啶基,2,2'-联吡啶或1,10-的反应菲咯啉在水热条件下(180°C / 15 h)产生高产率的复合物[MF 3(terpy)]·3H 2 O,[MF 3(bipy)(OH 2)]·2H 2 O和[MF 3( phen)(OH 2)]。[M'F 3(terpy )]·3H 2 O(M'= Al或Ga),[M'F 3(bipy)(OH 2)]·2H 2 O和[GaF 3(苯)(OH 2)]表明它们全部在金属上具有扭曲的八面体几何形状,且具有三氟化硫配位。广泛的H键(F⋯H–OH)连接分子。通过显微分析,IR,1 H,19 F 1 H}和27 Al NMR光谱进一步表征了该配合物。相反,在类似的水热条件下,三氟化物与无环三胺N,N,N ',N ',N ''-五甲基二亚乙基三胺的反应导致三胺裂解并闭环形成1