title: Synthesis of carbaalane halogen derivatives.
abstract: The carbaalane halogen derivatives [(AlX)(6)(AlNMe(3))(2)(CCH(2)CH(2)SiMe(3))(6)] (X = F (9), Cl (7), Br (10), I (11)) were prepared in toluene from [(AlH)(6)(AlNMe(3))(2)(CCH(2)CH(2)SiMe(3))(6)] (6) and BF(3).OEt(2), BX(3) (X = Br, I), Me(3)SnF, and Me(3)SiX (X = Cl, Br, I), respectively. A partially halogenated product [(AlH)(2)(AlX)(4)(AlNMe(3))(2)(CCH(2)CH(2)SiMe(3))(6)] (12) (X = Cl (approximately 40%), Br (approximately 60%)) was obtained from 5 and impure BBr(3). [(AlH)(6)(AlNMe(3))(2)(CCH(2)Ph)(6)] (5) was converted to [(AlX)(6)(AlNMe(3))(2)(CCH(2)Ph)(6)] (X = F (13), Cl (14), Br (15), I (16)) using BF(3).OEt(2) and Me(3)SiX (X = Cl, Br, I), respectively. The X-ray single-crystal structures of 11.C(6)H(6), 12.3C(7)H(8), 13.6C(7)H(8), and 15.4C(7)H(8) were determined. Compounds 7 and 9-11 are soluble in benzene/toluene and could be well characterized by NMR spectroscopy and MS (EI) spectrometry. The results demonstrate the facile substitution of the hydridic hydrogen atoms in 5 and 6 by the halides with different reagents.
authors.affiliation: Institut für Anorganische Chemie der Georg-August-Universität Göttingen, Tammannstrasse 4, D-37077 Goettingen, Germany.
authors.forename: Andreas
authors.initials: A
authors.lastname: Stasch
authors.forename: Herbert W
authors.initials: HW
authors.lastname: Roesky
authors.forename: Denis
authors.initials: D
authors.lastname: Vidovic
authors.forename: Jörg
authors.initials: J
authors.lastname: Magull
authors.forename: Hans-Georg
authors.initials: HG
authors.lastname: Schmidt
authors.forename: Mathias
authors.initials: M
authors.lastname: Noltemeyer