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Inorg Chem. 2000 Apr 03;39(7):1561-7. doi: 10.1021/ic990945l.

Syntheses and structures of methyltris(pyrazolyl)silane complexes of the group 6 metals.

Inorganic chemistry

E E Pullen, D Rabinovich, C D Incarvito, T E Concolino, A L Rheingold

Affiliations

  1. Department of Chemistry, University of North Carolina at Charlotte, 9201 University City Boulevard, Charlotte, North Carolina 28223, USA.

PMID: 12526465 DOI: 10.1021/ic990945l

Abstract

The methyltris(3,5-dimethylpyrazolyl)silane ligand, TpsMe2, was readily prepared by the metathesis reaction of methyltrichlorosilane with 3 equiv of lithium 3,5-dimethylpyrazolate. The octahedral tricarbonyl complexes (TpsMe2)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 isostructural and 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 (251-264 degrees) in (TpsMe2)M(CO)3 and also to estimate a value of 1.59 A for the covalent radius of octahedral W(0).

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