15283-71-3Relevant articles and documents
Ansa-titanocene catalysts for α-Olefin polymerization. Syntheses, structures, and reactions with methylaluminoxane and boron-based activators
Bryliakov, Konstantin P.,Babushkin, Dmitrii E.,Talsi, Evgenii P.,Voskoboynikov, Alexander Z.,Gritzo, Holger,Schroeder, Lars,Damrau, Hans-Robert H.,Wieser, Ulrich,Schaper, Frank,Brintzinger, Hans H.
, p. 894 - 904 (2005)
The racemic isomers of C2H4(1-Ind) 2TiCl2 and Me2Si(2-Me-Benzind) 2TiMe2 were synthesized and structurally characterized. Reactions of these and related ansa-titanocene complexes
Al22Cl20·12L (L = THF, THP): The first polyhedral aluminum chlorides
Klemp,Bruns,Gauss,Haeussermann,Stoesser,Van Wuellen,Jansen,Schnoeckel
, p. 9099 - 9106 (2007/10/03)
Aluminum subhalides of the type Al22X20·12L (X = Cl, Br; L = THF, THP) are the only known representatives of polyhedral aluminum subhalides and exhibit interesting multicenter bonding properties. Herein, we report on the synthesis an
New routes to synthetically useful, sterically encumbered arylaluminum halides and hydride halides
Wehmschulte, Rudolf J.,Power, Philip P.
, p. 3262 - 3267 (2008/10/09)
The synthesis and structural characterization of the compounds Mes*AlCl2(THF) (1), Mes*AlCl2 (2), Mes*Al(H)Cl(THF) (3a), Mes*Al(H)Cl (4a), and (Mes*AlH2): (5) (Mes* = 2,4,6-t-Bu3C6H2-) are described as well as those for two compounds 3b and 4b that are analogs of 3a and 4a but have H:Cl ratios that are less than 1:1. All compounds were characterized by 1H, 13C NMR, and IR spectroscopy, and 1, 2, 3a, and 4b were additionally characterized by X-ray crystallography. Compound 1 is best synthesized by the reaction of [(THF)2LiH3AlMes*]2 (6) with 6 equiv of Me3SiCl. A more conventional route involving the addition of (THF)2LiMes* to 2 equiv of AlCl3 in toluene usually affords a mixture of 1 and AlCl3·THF. Recrystallization of 1 from n-hexane results in a species that has less than 1 equiv of THF per Mes* AlCl2 The THF free complex 2 may be obtained in quantitative yield by heating 1 for 20 min at 90 °C under reduced pressure. Compound 3a may be obtained by treating a 1:1 mixture of Mes*Li(THF)2 and LiAlH4 with 2 equiv of Me30SiCl or by the addition of slightly less than 4 equiv of Me3SiCl to 6. The THF can be removed from 3a by sublimation to give 4a. The related compounds 3b and 4b, which display an aluminum-bound H:Cl ratio that is deficient in H, can be obtained by reactions with slightly more than 2 equiv of Me3SiCl. Crystal data at 130 K with Cu Kα (λ = 1.541 78 A?) radiation: 1, C22H37AlCl2O, a = 11.889(3) A?, b = 9.992(3) A? , c = 19.704(5) A?, orthorhombic, space group Pca21, Z = 4, R = 0.068 for 1556 (I > 2σ(I)) data; 2, C18H29AlCl2, a = 12.147(5) A?, b = 18.042(6) A?, c = 17.771(7) A?, β= 95.77(3)°, monoclinic, space group P21/n, Z = 8, R = 0.032 for 4610 (I > 2σa(I)} data; 3a, C22H38AlClO, a = 16.887(7) A?, b = 16.333(6) A?, c = 8.739(3) A?, β= 101.41(3)°, monoclinic, space group P21/c, Z = 4, R = 0.073 for 2752 (I > 2σ(I)) data; 4b, C18H29.64AlCl1.36, a = 12.077(3) A?, b = 17.920(3) A?, c = 17.634(5) A? ; β = 95.21(2) A?, monoclinic, space group P21/n, Z = 8, R = 0.070 for 4261 (I > 2σ(I)) data.
