A Pyridine‐Stabilized Alumoxane Containing Two 1,3,2‐Diazaalumina[3]ferrocenophane Units

2‐Chloro‐1,3‐bis(trimethylsilyl)‐1,3‐diaza‐2‐metalla‐[3]ferrocenophanes with M = Y (3) and Sc (4) have been prepared as the dipyridine adducts, starting from YCl3 and ScCl3, respectively, and N,N′‐dilithio‐N,N′‐bis(trimethylsilyl)‐1,1′‐diaminoferrocene (2). The reaction of 3 with sodium pentamethylcyclopentadienide (NaCp*) gave the complex 5, in which the yttrium atom is four‐coordinate, bearing the diamido ligand, Cp* and one pyridine ligand. An ate complex of four‐coordinate yttrium (6) was obtained, when YCl3 was treated with 2 equiv. of 2. In 6a, the lithium atom is threefold coordinated by two of the four amido nitrogen atoms and by pyridine, and addition of an excess of pyridine gave the separated ion pairs (6b) in solution. The molecular structures of 3, 5 and 6a were determined by X‐ray structural analysis, and the solution‐state structures were deduced from consistent NMR spectroscopic data sets (1H, 13C, 29Si, 89Y NMR). The 89Y nuclear magnetic shielding of amido complexes appears to increase with the coordination number (3, 4, 5) of yttrium.(© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008)

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Five‐ and Four‐Coordinate 1,3‐Diaza‐2‐yttria‐ and 1,3‐Diaza‐2‐scandia‐[3]ferrocenophanes

Wrackmeyer

Klimkina

Milius

2008

Eur J Inorg Chem

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Effect of the Nitrogen Substituent on the Reactions of Alane towards Imino‐ and Aminophenols: Generation of a Dinuclear Aluminoxane

2012

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AlH3·NEtMe2 reacts with salicylaldimines 3,5‐tBu2–2‐(OH)C6H2CH=NR [R = C6F5 (1a), 2,6‐Me2C6H3 (1b); 0.5 equiv.] to give the bisphenoxido‐amido‐imino compounds [Al{3,5‐tBu2–2‐(O)C6H2CH=NR}{3,5‐tBu2–2‐(O)C6H2CH2–NR}] [R = C6F5 (4a), 2,6‐Me2C6H3 (4b)]. When the substituent on the nitrogen is 2,6‐Me2C6H3, it is possible to isolate the bis(phenoxido‐imino) hydride [AlH{3,5‐tBu2–2‐(O)C6H2CH=N–2,6‐Me2C6H3}2] (3) if the reaction is performed at low temperature. Compound 4a is converted in wet toluene at room temperature readily and quantitatively into the aluminoxane [(Al{3,5‐tBu2–2‐(O)C6H2CH=NC6F5}{3,5‐tBu2–2‐(O)C6H2CH2–NHC6F5})2O] (5). The mononuclear bis(phenoxido‐amino) hydrides [AlH{3,5‐tBu2–2‐(O)C6H2CH2–NHR}2] [R = 2,6‐Me2C6H3 (6b), tBu (6c)] are obtained by treatment of AlH3·NEtMe2 with aminophenols 3,5‐tBu2–2‐(OH)C6H2CH2–NHR [R = 2,6‐Me2C6H3 (2b), tBu (2c); 0.5 equiv.] in toluene at –78 °C. Compound 6b evolves into [Al{3,5‐tBu2–2‐(O)C6H2CH2–NH–2,6‐Me2C6H3}{3,5‐tBu2–2‐(O)C6H2CH2–N–2,6‐Me2C6H3}] (7), which can also be generated by the direct reaction of 2b with AlH3·NEtMe2 (0.5 equiv.) at room temperature. The molecular structures of 4b and 5 have been determined by X‐ray diffraction analysis.

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Ferrocenophanes with Interannular Nitrogen–Gallium Bridges. 1,3,2‐Diazagalla‐[3]Ferrocenophanes and an 1‐Aza‐3‐Azonia‐2‐Gallata‐[3]Ferrocenophane. Synthesis and Structure

Wrackmeyer

Klimkina

Milius

2009

Zeitschrift anorg allge chemie

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1,1′‐Bis(trimethylsilylamino)ferrocene reacts with trimethyl‐ and triethylgallium to give the μ‐[ferrocene‐1,1′‐diyl‐bis(trimethylsilylamido)]tetraalkyldigallanes. These were converted into the 1,3‐bis(trimethylsilyl)‐2‐alkyl‐2‐pyridine‐1,3,2‐diazagalla‐[3]ferrocenophanes, of which the ethyl derivative was characterized by X‐ray structural analysis. Treatment of gallium trichloride with N,N′‐dilithio‐1,1′‐bis(trimethylsilylamino)ferrocene affords μ‐[ferrocene‐1,1′‐diyl‐bis(trimethylsilylamido)]tetrachlorodigallane along with bis(trimethylsilyl)‐2,2‐dichloro‐1‐aza‐3‐azonia‐2‐gallata‐[3]ferrocenophane as a side product, and both were structurally characterized by X‐ray analysis. The solution‐state structures of the new gallium compounds and aspects of their molecular dynamics in solution were studied by NMR spectroscopy (1H, 13C, 29Si NMR).

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A Pyridine‐Stabilized Alumoxane Containing Two 1,3,2‐Diazaalumina[3]ferrocenophane Units

Cited by 10 publications

References 49 publications

Five‐ and Four‐Coordinate 1,3‐Diaza‐2‐yttria‐ and 1,3‐Diaza‐2‐scandia‐[3]ferrocenophanes

Five‐ and Four‐Coordinate 1,3‐Diaza‐2‐yttria‐ and 1,3‐Diaza‐2‐scandia‐[3]ferrocenophanes

Effect of the Nitrogen Substituent on the Reactions of Alane towards Imino‐ and Aminophenols: Generation of a Dinuclear Aluminoxane

Ferrocenophanes with Interannular Nitrogen–Gallium Bridges. 1,3,2‐Diazagalla‐[3]Ferrocenophanes and an 1‐Aza‐3‐Azonia‐2‐Gallata‐[3]Ferrocenophane. Synthesis and Structure

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