GROUP-13 CHEMISTRY OF STERICALLY HINDERED AMINES - SYNTHESIS AND MOLECULAR-STRUCTURE OF (ME2M-ADA)2 (M=AL, GA - ADA=1-AMINOADAMANTANE) AND ((I-BU)AL-IMINODIBENZYL)2

被引:28
作者
LEE, BS [1 ]
PENNINGTON, WT [1 ]
ROBINSON, GH [1 ]
机构
[1] CLEMSON UNIV,DEPT CHEM,CLEMSON,SC 29634
关键词
D O I
10.1016/S0020-1693(00)80250-9
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Reaction of Me3M (M = Al, Ga) with 1-aminoadamantane, Ada, in toluene affords crystalline complexes of the type [Me2M-Ada]2. The gallium compound, I, isomorphous with the aluminum compound, II, crystallizes in the triclinic space group P1BAR with unit cell parameters a = 6.728(1), b = 9.957(2), c = 10.341(2) angstrom, alpha = 74.30(1), beta = 73.94(1), gamma = 72.19(1)-degrees, V = 620.6(2) angstrom 3 and D(calc) = 1.34 g cm-3 for Z = 1. Least-squares refinement based on 1794 observed reflections (I > 3-sigma(I)) converged at R = 0.059, R(w) = 0.080. I resides about a crystallographic center of symmetry and contains a planar Ga2N2 four-membered ring. The Ga2N2 ring has a mean Ga-N bond distance of 2.030(9) angstrom. The mean Ga-C bond distance in the dimethylgallium unit is 1.974(9) angstrom. The crystalline product [(i-Bu)Al-iminodibenzyl]2 (III), isolated from reaction of diisobutylaluminum hydride with iminodibenzyl, (C14H12)NH, in toluene, crystallizes in the triclinic space group P1BAR with unit cell parameters a = 10.767(2), b = 12.264(3), c = 13.230(4) angstrom, alpha = 75.57(2), beta = 74.14(2), gamma = 73.58(2)degrees, V = 1583.7(7) angstrom 3 and D(calc) = 1.16 g cm-3 for Z = 2. Least-squares refinement based on 2216 observed reflections (I > 3-sigma(I)) converged at R = 0.093, R(w) = 0.118. Compound III results from a unique condensation reaction in which ortho-metallation of one of the aromatic rings of iminodibenzyl was observed. Compound III has a mean Al-N bond distance of 2.036(7) angstrom. The mean Al-C(isobutyl) bond distance of 1.98(3) angstrom is comparable to 1.954(8) angstrom for the Al-C(aromatic) fragment.
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页码:173 / 178
页数:6
相关论文
共 24 条
  • [1] HASEN HD, 1979, J ORGANOMET CHEM, V175, P33
  • [2] CRYSTAL AND MOLECULAR-STRUCTURES OF DIMETHYLALUMINUM-N,N'-DIMETHYLACETAMIDINE AND DIMETHYLGALLIUM-N,N'-DIMETHYLACETAMIDINE DIMERS [(CH3)2M(NCH3)2CCH3]2 (M=AL,GA)
    HAUSEN, HD
    GERSTNER, F
    SCHWARZ, W
    [J]. JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1978, 145 (03) : 277 - 284
  • [3] HOBERG H, 1972, LIEBIGS ANN CHEM, V766, P142
  • [4] TRIMETHYLMETAL UROTROPINE ADDUCTS OF ALUMINUM, GALLIUM, INDIUM AND THALLIUM
    KRAUSE, H
    SILLE, K
    HAUSEN, HD
    WEIDLEIN, J
    [J]. JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1982, 235 (03) : 253 - 264
  • [5] LEE B, 1990, J ORGANOMET CHEM, V396, P296
  • [6] LEE B, 1991, INORG CHEM, V30, P809
  • [7] THE 1ST EXAMPLE OF A FERROCENYLGALLANE - SYNTHESIS, PROPERTIES, AND X-RAY CRYSTAL-STRUCTURE OF THE [(ETA-5-C5H5)FE(ETA-5-C5H4)GA(CH3)2]2 DIMER
    LEE, BS
    PENNINGTON, WT
    LASKE, JA
    ROBINSON, GH
    [J]. ORGANOMETALLICS, 1990, 9 (11) : 2864 - 2865
  • [8] POWER PP, 1988, ANGEW CHEM INT EDIT, V27, P1699
  • [9] CRYSTAL AND MOLECULAR-STRUCTURES OF PYRAZOLYLGALLIUM, 3-METHYLPYRAZOLYLGALLIUM, AND INDAZOLYLGALLIUM DIMETHYL DIMERS
    RENDLE, DF
    STORR, A
    TROTTER, J
    [J]. CANADIAN JOURNAL OF CHEMISTRY-REVUE CANADIENNE DE CHIMIE, 1975, 53 (19): : 2930 - 2943
  • [10] CRYSTAL AND MOLECULAR-STRUCTURES OF 3,5-DIMETHYLPYRAZOLYLGALLIUM DIMETHYL DIMER,[ME2GA.N2C5H7]2, AND HYDROXY-BRIDGED SPECIES, [ME2GA(OH)(N2C5H7)GAME2.2N2C5H8]
    RENDLE, DF
    STORR, A
    TROTTER, J
    [J]. CANADIAN JOURNAL OF CHEMISTRY-REVUE CANADIENNE DE CHIMIE, 1975, 53 (19): : 2944 - 2954