SYNTHESIS, STRUCTURE, AND PYROLYSIS OF ORGANOALUMINUM AMIDES DERIVED FROM THE REACTIONS OF TRIALKYLALUMINUM COMPOUNDS WITH ETHYLENEDIAMINE IN A 3-2 RATIO

被引:39
作者
JIANG, Z
INTERRANTE, LV
KWON, D
THAM, FS
KULLNIG, R
机构
[1] RENSSELAER POLYTECH INST,DEPT CHEM,TROY,NY 12180
[2] STERLING WINTHROP RES INST,RENSSELAER,NY 12144
关键词
D O I
10.1021/ic00005a023
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The reactions of triethylaluminum and trimethylaluminum with ethylenediamine (en) in a 3:2 ratio have been studied. Heating of the initially formed (R3Al)2.en and R3Al.en adduct mixture results in the formation of RAl[(HN(CH2)2NH)AIR2]2 (R = CH3 [3] and C2H5 [4]). The structures and formation mechanisms of these two compounds, as well as their pyrolysis reactions, have been studied with H-1, C-13, and Al-27 NMR, FTIR, MS, GC, DSC, and TGA techniques. The methyl derivative (3) was characterized by a single-crystal X-ray diffraction analysis: space group P2@c; a = 15.523 (3) angstrom; b = 8.419 (1) angstrom; c = 13.464 (3) angstrom; V = 1663.8 (5) angstrom-3; beta = 109.00 (2)-degrees; Z = 4. Full-matrix least-squares refinement converges as R = 0.051 and R(w) = 0.076 based on 2280 reflections with F > 4-sigma-(F). Both four- and five-coordinated Al atoms were observed in which the en-2H groups serve as both chelating and bridging ligands.
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页码:995 / 1000
页数:6
相关论文
共 19 条
  • [1] CHELATION IN ORGANOALUMINUM-NITROGEN CHEMISTRY
    BEACHLEY, OT
    RACETTE, KC
    [J]. INORGANIC CHEMISTRY, 1976, 15 (09) : 2110 - 2115
  • [2] BEACHLEY OT, 1974, INORG CHEM, V14, P2534
  • [3] AL-27-NMR SPECTROSCOPY - A PROBE FOR THREEFOLD, FOURFOLD, FIVEFOLD, AND SIXFOLD COORDINATED AL ATOMS IN ORGANO-ALUMINUM COMPOUNDS
    BENN, R
    RUFINSKA, A
    LEHMKUHL, H
    JANSSEN, E
    KRUGER, C
    [J]. ANGEWANDTE CHEMIE-INTERNATIONAL EDITION IN ENGLISH, 1983, 22 (10): : 779 - 780
  • [4] Organometallic Azides as Precursors for Aluminum Nitride Thin Films
    Boyd, David C.
    Haasch, Richard T.
    Mantell, Daniel R.
    Schulze, Roland K.
    Evans, John F.
    Gladfelter, Wayne L.
    [J]. CHEMISTRY OF MATERIALS, 1989, 1 (01) : 119 - 124
  • [5] HAHN T, 1983, INT TABLES CRYSTALLO, VA, P169
  • [6] Haiduc I., 1987, CHEM INORGANIC HOMO, P167
  • [7] Ibers J. A., 1974, INT TABLES XRAY CRYS, VIV, p[99, 149]
  • [8] Interrante L. V., 1986, MATER RES SOC S P, V73, P359
  • [9] N,N'-BIS(TRIETHYLALUMINIO)ETHYLENEDIAMINE-DERIVED AND N,N'-BIS(TRIMETHYLALUMINIO)ETHYLENEDIAMINE-DERIVED ORGANOMETALLIC PRECURSORS TO ALUMINUM NITRIDE - SYNTHESES, STRUCTURES, AND PYROLYSES
    JIANG, ZP
    INTERRANTE, LV
    [J]. CHEMISTRY OF MATERIALS, 1990, 2 (04) : 439 - 446
  • [10] KRIZ O, 1984, J MAGN RESON, V60, P375, DOI 10.1016/0022-2364(84)90048-9