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2. Tetraaza analogues of lithium and sodium alums: synthesis and X-ray structures of the single strand polymer [Li(THF)2(Al[SO2(NtBu)2]2)] infinity and the contact ion pairs [Na(15-crown-5)][Al(SO2(NtBu)2)2] and ([Na(15-crown-5)][O2S(mu-NBn)2Al(mu-NBnSO2NBn)])2

Author

P, Blais, J K, Brask, T, Chivers, and G, Schatte

Abstract

The reaction of an alkali metal aluminohydride MAlH4 (M = Li, Na) with N,N'-bis-(tert-butyl)sulfamide or N,N'-bis-(benzyl)sulfamide in THF produces the complex ions (Al[SO2(NR)2]2)- (R = tBu, Bn). The X-ray structures of [Li(THF)2(Al[SO2(NtBu)2]2)] infinity (1), [Na(15-crown-5)][Al(SO2(NtBu)2)2], (2) and ([Na(15-crown-5)][O2S(mu-NBn)2Al(mu-NBnSO2NBn)])2 (3.3THF) are reported. The two diazasulfate ligands [SO2(NtBu)2]2- are N,N' chelated to Al3+ in both 1 and 2. In the lithium derivative 1 the spirocyclic (Al[SO2(NtBu)2]2)- anions are bridged by the bis-solvated cations Li(THF)2+ to give a polymeric strand. In the sodium salt 2 the complex anion is O,O' chelated to Na+, which is further encapsulated by a 15-crown-5 ligand to give a monomeric ion-pair complex. By contrast, the benzyl derivative 3 forms a dimer in which the terminal [SO2(NBn)2]2- ligands are (N,N'),(O,O') bis-chelated to Al3+ and Na+, respectively, and the bridging ligands adopt a novel N,O-chelate, N'-monodentate bonding mode. The central core of 3 consists of two four-membered AlOSN rings bridged by two NtBu groups. Crystal data: 1, orthorhombic, Pna2(1), a = 20.159(5) degrees, b = 10.354(3) degrees, c = 15.833(4) degrees, alpha = beta = gamma = 90 degrees, V = 3304.7(15) A3, Z = 4; 2, monoclinic, P2(1)/n, a = 16.031(2) A, b = 9.907(2) A, c = 23.963(4) A, beta = 103.326(2) degrees, Z = 4; 3, triclinic, P1, a = 12.7237(11) A, b = 14.0108(13) A, c = 16.2050(14) A, alpha = 110.351(2) degrees, beta = 111.538(2) degrees, gamma = 97.350(2) degrees, Z = 1.

Published
2001

3. Group 13 Chemistry

Author

Pamela J. Shapiro, David A. Atwood, Ned J. Hardman, Andrew D. Phillips, Philip P. Power, L. O. Schebaum, P. Jutzi, Thomas P. Fehlner, Charles A. G. Carter, Kevin D. John, Grace Mann, Richard L. Martin, Thomas M. Cameron, R. Tom Baker, Karyn L. Bishop, Richard D. Broene, Stephen A. Westcott, John J. Eisch, Peter O. Otieno, Katrin Mackenzie, Boguslaw W. Kotowicz, Frieder Jäkle, François P. Gabbaï, Melanie J. Harvey, Peter H. M. Budzelaar, Giovanni Talarico, Hansgeorg Schnöckel, Andreas Schnepf, Mark J. Pender, Kersten M. Forsthoefel, Larry G. Sneddon, Mark R. Mason, R. Mark Matthews, Alisa M. Perkins, Vira V. Ponomarova, P. Blais, J. K. Brask, T. Chivers, C. Fedorchuk, G. Schatte, R. B. King, I. Silaghi-Dumitrescu, A. Kun, S. Anitha, P. Shanmugavelu, Valeswara-Rao Gazula, S. K. Shankar, Rani B. Menon, R. V. Rao, Jagannatha K. S. Rao, Luigi Zecca, C. Y. Wang, S. P. Bi, M. B. Luo, B. D. Conley, U. Dutta, C. Fridh, A. L. Gilliam, B. C. Yearwood, J. P. Selegue, D. A. Atwood, Anna Strunecka, Jiri Patocka, Pamela J. Shapiro, David A. Atwood, Ned J. Hardman, Andrew D. Phillips, Philip P. Power, L. O. Schebaum, P. Jutzi, Thomas P. Fehlner, Charles A. G. Carter, Kevin D. John, Grace Mann, Richard L. Martin, Thomas M. Cameron, R. Tom Baker, Karyn L. Bishop, Richard D. Broene, Stephen A. Westcott, John J. Eisch, Peter O. Otieno, Katrin Mackenzie, Boguslaw W. Kotowicz, Frieder Jäkle, François P. Gabbaï, Melanie J. Harvey, Peter H. M. Budzelaar, Giovanni Talarico, Hansgeorg Schnöckel, Andreas Schnepf, Mark J. Pender, Kersten M. Forsthoefel, Larry G. Sneddon, Mark R. Mason, R. Mark Matthews, Alisa M. Perkins, Vira V. Ponomarova, P. Blais, J. K. Brask, T. Chivers, C. Fedorchuk, G. Schatte, R. B. King, I. Silaghi-Dumitrescu, A. Kun, S. Anitha, P. Shanmugavelu, Valeswara-Rao Gazula, S. K. Shankar, Rani B. Menon, R. V. Rao, Jagannatha K. S. Rao, Luigi Zecca, C. Y. Wang, S. P. Bi, M. B. Luo, B. D. Conley, U. Dutta, C. Fridh, A. L. Gilliam, B. C. Yearwood, J. P. Selegue, D. A. Atwood, Anna Strunecka, and Jiri Patocka

Published
2002

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