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).
The one-dimensional copper(I) coordination polymers Cu(3){MeSi(CH(2)SMe)(3)}(2)X(3) (X = Cl, Br) and [{MeSi(CH(2)SMe)(3)}Cu(NCMe)]Y (Y = OSO(2)CF(3), BF(4), PF(6)) were readily obtained in very good to excellent yields (80-95%) by reacting CuX or [Cu(NCMe)(4)]Y, respectively, with the tridentate thioether ligand MeSi(CH(2)SMe)(3) in acetonitrile. The new complexes were characterized by a combination of analytical and spectroscopic techniques, including electrospray ionization mass spectrometry and, for the bromo and hexafluorophosphate derivatives, single-crystal X-ray diffraction. Both complexes exhibit one-dimensional chain structures with approximately tetrahedral copper centers and bridging unidentate/bidentate thioether ligands.
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