Syntheses and Structures of Methyltris(pyrazolyl)silane Complexes of the Group 6 Metals

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• 作者：Eric E. Pullen ; Daniel Rabinovich ; Christopher D. Incarvito ; Thomas E. Concolino ; and Arnold L. Rheingold
• 刊名：Inorganic Chemistry
• 出版年：2000
• 出版时间：April 3, 2000
• 年：2000
• 卷：39
• 期：7
• 页码：1561 - 1567
• 全文大小：75K
• 年卷期：v.39,no.7(April 3, 2000)
• ISSN：1520-510X

文摘

The methyltris(3,5-dimethylpyrazolyl)silane ligand, Tps^Me₂, was readily prepared by the metathesis reaction ofmethyltrichlorosilane with 3 equiv of lithium 3,5-dimethylpyrazolate. The octahedral tricarbonyl complexes(Tps^Me₂)M(CO)₃ were synthesized either by ligand exchange with the labile nitrile adducts M(CO)₃(NCR)₃ (M =Cr, Mo, R = Me; M = W, R = Et) or thermally by direct substitution on the hexacarbonyls M(CO)₆ (M = Cr,Mo). The three new complexes were characterized by a combination of analytical and spectroscopic techniques,including electrospray ionization mass spectrometry and single-crystal X-ray diffraction. They are all isostructuraland display in the solid state the expected distorted octahedral geometries with facially coordinated tris(pyrazolyl)silane ligands. Crystallographic data were used to calculate the ligand cone angles (251-264es/entities/deg.gif">) in (Tps^Me₂)M(CO)₃ and also to estimate a value of 1.59 Å for the covalent radius of octahedral W(0).