3 years ago

Spontaneous vs. Base-Induced Dehydrochlorination of Group 14 ortho-Carboranylamidinates

Spontaneous vs. Base-Induced Dehydrochlorination of Group 14 ortho-Carboranylamidinates
Sabine Busse, Nicole Harmgarth, Liane Hilfert, Frank T. Edelmann, Phil Liebing, Andreas Förster
The reaction of the lithium ortho-carboranylamidinate Li[HL] {HL = [o-C2B10H10C(NiPr)(NHiPr)]} with ECl2R2 (E = Si, Ge, Sn, Pb; R = Cl, Me, Bu, Ph) leads to new ortho-carboranylamidinates of the group 14 elements. In the case of the heavier elements, Ge, Sn, and Pb, compounds of the composition R2ECl[HL] were obtained in a straightforward manner, where the E atom adopts trigonal-bipyramidal coordination. In the case of Si, disproportionation to R2Si[L] and H2L takes place immediately. The R2Si[L]-type compounds, in which the Si atom exhibits a tetrahedral coordination, were obtained in a targeted synthesis protocol by reaction of the doubly lithiated ligand Li2L with R2SiCl2. The heavier homologues Cl2Ge[L] and Cl2Sn[L](THF) have been obtained accordingly. In contrast, it was found that deprotonation of R2ECl[HL] to R2E[L], employing triethylamine as a base, is not appropriate. All new compounds have been characterized by single-crystal X-ray diffraction, IR spectroscopy, and NMR spectroscopy, as well as mass spectrometry. Compounds of the types R2ECl[HL] and R2E[L] {E = Si, Ge, Sn, Pb; HL = [o-C2B10H10C(NiPr)(NHiPr)]} are described. The stability of R2ECl[HL] increases on going from Si to Pb.

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

DOI: 10.1002/ejic.201700500

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