3 years ago

Yttrium Methanide and Methanediide Bis(silyl)amide Complexes

Yttrium Methanide and Methanediide Bis(silyl)amide Complexes
Stephen T. Liddle, Matthew Gregson, David P. Mills, Fabrizio Ortu, Ashley J. Wooles
The yttrium methanediide complex [Y(BIPM)(I)(THF)2] (BIPM = {C(PPh2NSiMe3)2}) was reacted with a series of potassium bis(silyl)amides to produce heteroleptic complexes by salt metathesis protocols. The methanediide complexes [Y(BIPM)(N″)(THF)] (1; N″ = {N(SiMe3)2}) and [Y(BIPM)(N**)(THF)] (2; N** = {N(SiMe2tBu)2}) were obtained for those relatively small bis(silyl)amides. Complex 2 undergoes thermal decomposition under vacuum to yield the methanide cyclometalate complex [Y(H-BIPM){N(SitBuMe2)(SitBuMeCH2)-κ2-N,C}] (3) as part of an otherwise intractable mixture of products. Complex 3 was also observed in trace amounts in mixtures of [Y(BIPM)(I)(THF)2] and KN**. In contrast, [Y(BIPM)(I)(THF)2] reacted with the more sterically demanding potassium bis(silyl)amides KN* (N* = {N(SiMe2tBu)(SiiPr3)}) and KN†† (N†† = {N(SiiPr3)2}) to afford the methanide cyclometalate complexes [Y(H-BIPM){N(SiiPr3)(SitBuMeCH2)-κ2-N,C)}] (4) and [Y(H-BIPM){N(SiiPr3)[SiiPr2(CHMeCH2)]-κ2-N,C}] (5), respectively. Complexes 15 were characterized as appropriate by multinuclear NMR and FTIR spectroscopy, elemental analyses, and single-crystal X-ray diffraction.

Publisher URL: http://dx.doi.org/10.1021/acs.organomet.7b00394

DOI: 10.1021/acs.organomet.7b00394

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