Joseph Q. Nguyen, Lauren M. Anderson-Sanchez, Joseph W. Ziller and William J. Evans*,
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引用次数: 0
Abstract
Despite the importance of bis(cyclopentadienyl) scandium(III) halide complexes as precursors in the development of scandium metallocene chemistry, relatively few examples of this class have been structurally characterized. Since the cyclopentadienyl ring substitution pattern and the halide identity can have a major influence on organoscandium complex synthesis and reactivity, it is critical to have a variety of well-characterized [(C5R5)2ScX]n starting materials (R = H, alkyl, silyl; X = halide) available for exploration of this area. To remedy this deficiency, reactions between ScX3 (X = Cl and I) and 2 equiv of a variety of potassium cyclopentadienide reagents have been examined. This has provided, in good crystalline yield, the compounds [C5H3(SiMe3)2]2ScI, [C5Me4(SiMe3)]2ScI, [C5Me4(SiMe2tBu)]2ScI, {[C5H4(SiMe3)]2Sc(μ-I)}2, {[C5H4(SiiPr3)]2Sc(μ-I)}2, and {[C5H3(SiMe3)2]2Sc(μ-Cl)}2, each of which has been characterized by X-ray crystallography, elemental analysis, NMR spectroscopy (1H, 13C{1H}, 29Si{1H}, and 45Sc), and infrared spectroscopy. The study has also revealed the facile cocrystallization of the oxide {[C5H3(SiMe3)2]2Sc}2(μ-O) and hydroxide {[C5H3(SiMe3)2]2Sc(μ-OH)}2 impurities from preparations of [C5H3(SiMe3)2]2ScI using samples of ScI3 that presumably contain an oxide contaminant.
期刊介绍:
Organometallics is the flagship journal of organometallic chemistry and records progress in one of the most active fields of science, bridging organic and inorganic chemistry. The journal publishes Articles, Communications, Reviews, and Tutorials (instructional overviews) that depict research on the synthesis, structure, bonding, chemical reactivity, and reaction mechanisms for a variety of applications, including catalyst design and catalytic processes; main-group, transition-metal, and lanthanide and actinide metal chemistry; synthetic aspects of polymer science and materials science; and bioorganometallic chemistry.