Preparation of cyclopentadienyl molybdenum clusters linked by a cyclotetradeca-1,8-diyne ligand
Resource
Inorganica Chimica Acta 294 (2): 232-239
Journal
Inorganica Chimica Acta
Pages
232-239
Date Issued
1999
Date
1999
Author(s)
Abstract
The diyne-bridged complexes Cp2Mo2(CO)4(μ-η2-C14H20) (1) and [Cp2Mo2(CO)4]2(μ,μ-η 2,η2-C14H20) (2) have been prepared from the reactions of cyclotetradeca-1,8-diyne (C14H20) with Cp2Mo2(CO)6 in refluxing toluene, or with Cp2Mo2(CO)4 at 25°C. In contrast, Cp2Mo2(CO)6 reacts with Ag+BF4- and C14H20 to yield [CpMo+(CO)(μ,μ-η2,η2-C 14H20)]2(BF4-) 2 (3-BF4) through redox cleavage of the Mo-Mo bond. An alternative method to prepare 3-BF4 is via iodide abstraction of CpMoI(CO)3 by Ag+BF4- in the presence of C14H20. Compound 3-BF4 reacts with Me3NO in acetonitrile to afford [CpMo+(NCMe)(μ,μ-η2,n2-C 14H20)]2(BF4-) 2 (4-BF4). An alkyne-alkyne coupling reaction is achieved by treating 3-BF4 with PPN+Cl- to yield the cyclobutadienophane complex CpMo(CO)Cl(η4-C4(C10H20)) (5). Metathesis of 3-BF4 with Na+BPh4- gives [CpMo+(CO)(μ,μ-η2η2-C 14H20)]2(BPh4-) 2 (3-BPH4), the crystal structure of which was determined by X-ray diffraction. © 1999 Elsevier Science S.A. All rights reserved.
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