Organometallics, Journal Year: 2024, Volume and Issue: 44(1), P. 137 - 147
Published: Dec. 18, 2024
Despite the importance of bis(cyclopentadienyl) scandium(III) halide complexes as precursors in development scandium metallocene chemistry, relatively few examples this class have been structurally characterized. Since cyclopentadienyl ring substitution pattern and identity can a major influence on organoscandium complex synthesis reactivity, it is critical to variety well-characterized [(C5R5)2ScX]n starting materials (R = H, alkyl, silyl; X halide) available for exploration area. To remedy deficiency, reactions between ScX3 (X Cl I) 2 equiv potassium cyclopentadienide reagents examined. This has provided, good crystalline yield, compounds [C5H3(SiMe3)2]2ScI, [C5Me4(SiMe3)]2ScI, [C5Me4(SiMe2tBu)]2ScI, {[C5H4(SiMe3)]2Sc(μ-I)}2, {[C5H4(SiiPr3)]2Sc(μ-I)}2, {[C5H3(SiMe3)2]2Sc(μ-Cl)}2, each which characterized by X-ray crystallography, elemental analysis, NMR spectroscopy (1H, 13C{1H}, 29Si{1H}, 45Sc), infrared spectroscopy. The study also revealed facile cocrystallization oxide {[C5H3(SiMe3)2]2Sc}2(μ-O) hydroxide {[C5H3(SiMe3)2]2Sc(μ-OH)}2 impurities from preparations [C5H3(SiMe3)2]2ScI using samples ScI3 that presumably contain an contaminant.
Language: Английский