The Mg and Ca complexes of the tert-butyl substituted bis(amido)diazadiarsetidinides [{(tBuNAs) 2 (tBuN) 2 }M(thf) 2 ] (M = Mg (1), Ca (6)) were prepared by addition of nBu-secBuMg or [{(p-tBu)(C 6 H 4 )CH 2 } 2 Ca] to [(tBuNAs) 2 (tBuNH) 2 ] (Ia). Upon evaporation of coordinating THF, 1 is selectively converted to the amido(imino)arsenide complex [Mg{As(NtBu) 2 } 2 ] (2) whereas 6 decomposes to several products under these conditions. Hydrolysis of 2 with H 2 O yields the hitherto unknown

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... und As(NHtBu) 3 (3) whereas hydrolysis of Ia leads to the formation of the oxygen bridged bis(amidodiazadiarsetidine) [O {(tBuNH)(tBuNAs) 2 } 2 ] (4). Reaction of 2 with 3 yields the heteroleptic Mg complex with an amido(imino)arsenide and a bis(amido)diazadiarsetidinide ligand [{(tBuNAs) 2 (NHtBu)(NtBu)} Mg{As(NtBu) 2 }] (5). The homologous Ca compound ( 7 ) was obtained by conversion of Ia with Ca(hmds) 2 (hmds = N(SiMe 3 ) 2 ). Finally, the tetrylene complexes [E{(tBuNAs) 2 (tBuN) 2 }] (E = Ge (8), Sn (9), Pb (10)) were prepared by either conversion of Ia with E(hmds) 2 for E = Sn, Pb or by addition of the dichlorides of Ge and Sn to [(tBuNAs) 2 (tBuNLi) 2 ] (Ib). All compounds were characterised by NMR and IR spectroscopy, mass spectrometry and single crystal x-ray diffraction for 1, 2, 4, 5, 6 and 10.