4 years ago

Synthesis and Structural Characterization of Homo- and Heterometallic Li and Li/Ln Disiloxanediolate Complexes

Synthesis and Structural Characterization of Homo- and Heterometallic Li and Li/Ln Disiloxanediolate Complexes
Sabine Busse, Asim Ali, Liane Hilfert, Volker Lorenz, Frank T. Edelmann, Phil Liebing, Patrick Groß, Cristian G. Hrib, Janek Rausch
A series of new homo- and heterometallic lithium and lithium/lanthanide disiloxanediolate complexes were prepared and fully characterized. Three new adducts of dilithium tetraphenyldisiloxanediolate, [(Ph2SiOLi)2O] (2), with simple Lewis bases (Et2O, THF, DME) were prepared by treatment of Ph2Si(OH)OSiPh2(OH) (1) with 2 equiv. of n-butyllithium in the respective donor solvent. This way the adducts [{Ph2SiOLi(Et2O)}2O]2 (3), [{Ph2SiOLi(THF)}2O]2 (4), and [{Ph4Si2O(OLi)2}2(DME)3]∞ (5a) were obtained in a straightforward manner and in nearly quantitative yields. Treatment of anhydrous lanthanide(III) chlorides LnCl3 (Ln = Tb, Lu) with 2 equiv. of 2 in THF afforded the new lanthanide(III) bis(disiloxanediolate) complexes [{(Ph2SiO)2O}2{Li(THF)2}2]TbCl (6) and [{(Ph2SiO)2O}2{Li(THF)2}2]LuCl (7) in high yields. Similar reactions of LnCl3 (Ln = Ce, Nd) with 3 equiv. of 2 provided the heterometallic Li/Ln tris(disiloxanediolate) complexes [{(Ph2SiO)2O}3{Li(DME)}2{Li(THF)}]Ce (8) and [{(Ph2SiO)2O}3{Li(DME)}{Li(Et2O)}{Li(THF)}]Nd (9). All title compounds were structurally characterized through single-crystal X-ray diffraction.

Publisher URL: http://onlinelibrary.wiley.com/resolve/doi

DOI: 10.1002/zaac.201700324

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