Synthesis and reactions of aluminum hydride derivatives

Cucinella, S.; Mazzel, A.; Marconl, W

doi:10.1016/0073-8085(70)80012-2

Cited by 40 publications

(7 citation statements)

References 97 publications

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“…Yield: 3.01 g (74% based upon TMEDA). 1 H NMR (CD 2 Cl 2 , 400 MHz); δ ( ppm) = 3.243 (br, 3H, AlH 3 , FWHM = 17.323 Hz), 2.516 (s, 4H, N-CH 2 ), 2.270 (s, 12H, CH 3 ). 27 Al NMR (C 6 D 6 , 76 MHz); δ ( ppm) = 62.363 (FWHM = 5206.68 Hz).…”

Section: Synthesis and Characterisationmentioning

confidence: 99%

“…Yield: 12.51 g (84% based upon AlCl 3 ). 1 H NMR (C 6 D 6 , 300 MHz); δ ( ppm) = 4.238 (br, 3H, AlH 3 , FWHM = 81.226 Hz), 2.369 (qr, J = 7.3 Hz, 6H, N-CH 2 ), 0.862 (t, J = 7.3 Hz, 9H, CH 3 ). 27 Al NMR (C 6 H 6 , 76 MHz); δ ( ppm) = 142.168 (FWHM = 998.977 Hz).…”

Section: Synthesis and Characterisationmentioning

confidence: 99%

“…Yield: 2.30 g (14% based upon AlCl 3 ). 1 H NMR (C 6 D 6 , 300 MHz); δ ( ppm) = 7.09 (m, 5H, C 6 H 5 ), 4.05 (br, 3H, AlH 3 , FWHM = 103.097 Hz), 3.73 (s, 4H, N-CH 2 ), 2.13 (s, 6H, N-CH 3 ). 27 Al NMR (C 6 H 6 , 76 MHz); δ ( ppm) = 128.349 (FWHM = 5696.43 Hz.…”

Section: Synthesis and Characterisationmentioning

confidence: 99%

“…Yield: 1.55 g, 24% based upon TMPDA. 1 H NMR (CD 2 Cl 2 , 400 MHz); δ ( ppm) = 3.13 (br, 3H, AlH 3 , FWHM = 117.546 Hz), 2.42 (t, J = 7.9 Hz, 4H, N-CH 2 ), 2.28 (s, 12H, CH 3 ), 2.00 (m, J = 7.9 Hz, 2H, CH 2 CH 2 ). 27 Al NMR (CH 2 Cl 2 , 76 MHz); δ ( ppm) = 115.983 (FWHM = 996.058 Hz).…”

Section: Synthesis and Characterisationmentioning

confidence: 99%

“…The binary hydride of aluminium, AlH 3 or alane, is a sterically and electronically unsaturated moiety that reacts readily with a range of Lewis donors, leading to 1 : 1 and 1 : 2 adducts which are respectively four-or five-coordinate at the Al centre. [1][2][3] A wide range of such adducts have been synthesised and characterised over the past six decades, with ligands including carbenes, [4][5][6] phosphines, [7][8][9] amines, 10-13 ethers [14][15][16] and other oxygen donor molecules. 17 The four-coordinate 1 : 1 adducts of alane (AlH 3 •L) generally adopt a pseudo-tetrahedral configuration at the metal centre.…”

Section: Introductionmentioning

confidence: 99%

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Lewis base complexes of AlH3: structural determination of monomeric and polymeric adducts by X-ray crystallography and DFT calculations

et al. 2013

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The AlH3 adducts of TMEDA (Me2NCH2CH2NMe2), DIOX (O(CH2CH2)2O), TEA (Et3N), BDMA (PhNMe2), and TMPDA (Me2NCH2CH2CH2NMe2) have each been characterised by single-crystal X-ray diffraction at low temperature, by (1)H, (14)N and (27)Al NMR and FT-Raman and FT-IR spectroscopy, and by DFT calculations and elemental analysis. Hence, AlH3·TMEDA and AlH3·DIOX are both shown to adopt a polymeric structure, with the bidentate ligand bridging two Al centres, each of which adopts a trigonal bipyramidal (TBP) arrangement with equatorial hydride moieties. The 1 : 2 adduct AlH3·2BDMA is monomeric but the geometry at the Al centre resembles closely that of the polymeric TMEDA and DIOX complexes. AlH3·TEA alone adopts a monomeric structure in which the Al centre is tetrahedrally coordinated by three hydride and one amine ligand. The Al-L bond distance of 2.0240(17) Å for AlH3·TEA is the shortest of all the complexes in this study, and AlH3·TEA also possesses the shortest Al-H bonds. AlH3·DIOX has the shortest Al-L bond distance of the polymeric species (2.107(14) Å) on account of the higher electronegativity of the oxygen donor. The structure of AlH3·TMEDA was determined at low temperature (monoclinic space group P2(1)/c), and salient features are compared to the previous room temperature study, for which a highly disordered orthorhombic space group (P2(1)2(1)2(1)) was reported. The polymeric structures appear to be stabilised by a number of intermolecular interactions and unconventional hydrogen bonds; these are most pronounced for AlH3·DIOX, whose chains are connected by highly directional C-H···H-Al bonding with an H···H distance of 2.32(6) Å.

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Section: Synthesis and Characterisationmentioning

confidence: 99%

Section: Synthesis and Characterisationmentioning

confidence: 99%