Abstract
The title compounds were synthesized by the addition of AlMe3 to the corresponding azide suspended in an aromatic solvent. Both products were obtained as air-sensitive colorless crystals. Cs[Al2Me6N3]·2p-xylene crystallizes in the monoclinic space groupC2/m witha=19.143(6),b=16.227(6),c=10.392(5) Å, β=114.06(2)o, and ρcalc = 1.20 g cm−3 forZ=4. Refinement led to a conventionalR value of 0.037 for 2179 observed reflections. The cesium atom resides on a mirror plane, and the anion is disordered about a twofold axis. Thep-xylene molecules sandwich the cesium ion.
[K·dibenzo-18-crown-6] [AlMe6N3]·1.5(1-methylnaphthalene) crystallizes in the monoclinic space groupP21/c witha=14.176(5),b=13.021(5),c=25.324(8) Å, β=98.23(4)0, and ρcalc = 1.08 g cm−3 forZ=4. The finalR value was 0.132 for 1402 observed reflections. One of the 1-methylnaphthalene molecules is disordered about a center of inversion and interacts with the potassium ion. The other solvent molecule is found roughly in layers in the lattice and also exhibits disorder of the methyl substituent. For both title compounds the AlMe3 groups of the anion exhibit a staggered (C s) conformation.
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Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82015 (32 pages).
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Atwood, J.L., Hunter, W.E., Rogers, R.D. et al. Behavior of M[Al2Me6N3] (M=K, Rb, Cs) with aromatic solvents and the crystal structures of Cs[Al2Me6N3]·2p-xylene and [K·dibenzo-18-crown-6] [Al2Me6N3]· 1.5(1-methylnaphthalene). Journal of Inclusion Phenomena 3, 113–123 (1985). https://doi.org/10.1007/BF00687984
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DOI: https://doi.org/10.1007/BF00687984