1998
DOI: 10.1021/om980403w
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Synthesis and Characterization of an Orthometalated Aminoalane, [MeAlN(CH2Ph)-μ-(CH2C6H4)]2:  Molecular Structures of [MeAlN(CH2Ph)-μ-(CH2C6H4)]2 and [Me2AlN(CH2Ph)2]2

Abstract: Thermolysis of Me3Al with HN(CH2Ph)2 in toluene solution at 150 °C yields the orthometalated dimer [MeAlN(CH2Ph)-μ-(CH2C6H4)]2 (1) via the stepwise elimination of CH4. The molecular structure of 1 and that of the related aminoalane dimer [Me2AlN(CH2Ph)2]2 (2) were determined by single-crystal X-ray diffraction techniques. Complete 1H and 13C NMR chemical shift assignments for 1 were facilitated by the comparison of 1H NMR 2-D NOESY and X-ray distance data.

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Cited by 13 publications
(19 citation statements)
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“…The crystals melt to a deep red between 142Ϫ144°C and, as would be expected, Figure 2. Molecular structure of (S,S)-2; thermal ellipsoids shown at 50% probability; all H atoms omitted for clarity; selected bond length (Å ) and angles (°); Li(1)ϪN(3) 2.014 (12), Li(1)ϪN(4) 2.117 (14), Li(1)ϪN (5) Complex 2 crystallises in the orthorhombic space group P2 1 2 1 2 1 with four molecules in the unit cell. Although the crystal quality was not exceptionally high, leading to a large amount of weak intensities and high R int value, the structural solution was of sufficient quality to allow us to assign definitive atom connectivities.…”
Section: Resultsmentioning
confidence: 99%
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“…The crystals melt to a deep red between 142Ϫ144°C and, as would be expected, Figure 2. Molecular structure of (S,S)-2; thermal ellipsoids shown at 50% probability; all H atoms omitted for clarity; selected bond length (Å ) and angles (°); Li(1)ϪN(3) 2.014 (12), Li(1)ϪN(4) 2.117 (14), Li(1)ϪN (5) Complex 2 crystallises in the orthorhombic space group P2 1 2 1 2 1 with four molecules in the unit cell. Although the crystal quality was not exceptionally high, leading to a large amount of weak intensities and high R int value, the structural solution was of sufficient quality to allow us to assign definitive atom connectivities.…”
Section: Resultsmentioning
confidence: 99%
“…As can be seen, the Li cation, with its accompanying pmdta molecule, migrates from one N in the pyrazine ring in 1 to the opposite one in 2 as the lithium aluminate is formed. The Li(1)ϪO(2) bond at 2.543(11) Å would be considered long, however, an analysis of the bond angles at the sp 2 pyrazine nitrogen attached to Li reveals a high degree of asymmetry [Li(1)ϪN(3)ϪC (22) 108.7(5)°, Li(1)ϪN(3)ϪC (21) 136.4 (5) [14] while the bond from Al(1)ϪN(2) is longer than that commonly found {e.g. 1.934(2) Å in [Me 2 Al(Bn 2 N) 2 ]Li·(py)]}.…”
Section: Resultsmentioning
confidence: 99%
“…Triethylamine, chloro(trimethyl)silane, lithium aluminium hydride, pivaloyl chloride, AlMe 3 , AlCl 3 and n-butyllithium in hexanes (1.6 mol dm Ϫ3 , FMC corporation) were commercial samples used without further purification. The NMR solution spectra were recorded on Bruker DPX 300 (for 1 H and 13 C) or AMX 500 (for 29 Si and 27 Al) instruments and referenced externally (using aqueous Al(OH) 3 with a D 2 O lock for 27 Al or SiMe 4 for 29 Si) or internally ( 1 H, 13 C) to the residual solvent resonances; chemical shift data in δ. Unless otherwise stated, all NMR spectra were examined at 293 K in C 6 D 6 and, except for 1 H, were proton decoupled.…”
Section: Methodsmentioning
confidence: 99%
“…The remaining solid was dissolved in hexane and first frozen in liquid N 2 and then stored at Ϫ25 ЊC for several days to afford 9 as a beige solid (1.85 g, 49%) (it was too labile for elemental analysis), mp 45-50 ЊC (decomp.). 1 H NMR: δ 0.89 (s, 9H, Bu t ), 3.05 (vbr quartet, 4H, CH 2 ), 6.49-6.54 (m, 4H, Ph); 1 H NMR (343 K): δ 0.92 (s, 9H, Bu t ), 2.99, 3.02, 3.12, 3.15 (AB-type, 4H, CH 2 ), 6.54-6.59 (m, 4H, Ph); 13 C NMR (343 K): δ 29.83 (CMe 3 ), 34.17 (CMe 3 ), 59.52 (CH 2 ), 117.8, 120.75, 140.93 (Ph); 27 Al NMR: δ 115.2 ∆w ½ 3 kHz. MS (m/z, %): 273 (6%, [M Ϫ Cl] ϩ ).…”
Section: Crystallographymentioning
confidence: 99%
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