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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 4 (1986), S. 247-253 
    ISSN: 1573-1111
    Keywords: calix[8]arene ; crystal structure ; CDCl3 guest
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The methyl ether of calix[8]arene crystallizes from CDCl3 with two molecules of the solvent per molecule of host. An X-ray structural investigation has shown that the CDCl3 guests exist within the calixarene framework. The complex resides on a crystallographic center of inversion, and the cavity is roughly circular in projection as measured by the distance between centroids of aromatic rings related by the center: 14.5, 13.9, 10.1, and 11.2 Å. Six of the oxygen atoms are found on the inside and two on the outside. Crystals belong to the triclinic space group $$P\bar 1$$ witha=11.741(9),b=11.810(9),c=12.484(8) Å, α=94.74(8), β=104.41(8), γ=111.30(9)°, andD c =1.31 g cm−3 forZ=1. Refinement led to a finalR value of 0.086 for 949 observed reflections.
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  • 2
    ISSN: 1573-1111
    Keywords: Calix[8]arene ; crystal structure ; AlMe3 ; aromatic adduct
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Reaction of the methyl ether of calix[8]arene with AlMe3 yields [calix[8]arene methyl ether] [AlMe3]6·2 toluene,1, while that ofp-tert-butylcalix[8]arene gives [p-tert-butylcalix[8]arene methyl ether] [AlMe3]6·4 benzene,2. Both compounds1 and2 fail to react with alkali metal salts, MX. In1, the absence of a butylpara-substituent affords greater flexibility than is the case for thetert-butyl compound2. Thus, all six of the AlMe3 groups are located on the outside of the macrocyclic ring (in projection) in1, but two AlMe3 units are found on the inside in2. Colorless, air-sensitive crystals of1 belong to the triclinic space group $$P\bar 1$$ witha=13.690(8),b=14.317(4),c=14.738(6) Å, α=76.11(3), β=62.36(4), γ=82.41(4)o, andD c =1.06 g cm−3 forZ=1. Refinement led toR=0.101 for 1154 observed reflections.2 crystallizes in $$P\bar 1$$ with α=12.400(6),b=16.229(8),c=19.251(5) Å, α=96.17(3), β=107.25(3), γ=101.54(3)o, andD c =1.01 g cm−3 forZ=1. Refinement of2 gaveR=0.128 for 4351 observed reflections. The macrocyclic array in both1 and2 lies about a crystallographic center of inversion.
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  • 3
    ISSN: 1573-1111
    Keywords: Calix[4]arene ; aluminum alkyl ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The configurations of calix[4]arenes may be modified by the formation of donor-acceptor complexes which make use of the basicity of the oxygen atoms of the macrocycle. The complex [t-butylcalix[4]arene methyl ether][AlMe3]2,2, exhibits the previously unseen ‘1,2-alternate’ geometry, while [t-butylcalix[4]arene methyl ether][MeAlCl2]2,3, and [t-butylcalix[4]arene methyl ether][EtAlCl2]2,4, show the ‘1,3-alternate’ configuration.2 crystallizes in the triclinic space groupPl witha=11.14(1),b=11.60(1),c=12.02(1) Å, α=77.32(8), β=67.91(8), and γ=69.34(8)o withD c =1.06 g cm−3 forZ=1. Refinement based on 1270 observed reflections led toR=0.106.3 as the benzene solvate belongs to the monoclinic space groupC2/c witha=12.116(2),b=21.557(7),c=23.470(6) Å, and β=104.05(2)o withD c =1.13 g cm−3 forZ=4. Refinement based on 2335 observed reflections led toR=0.075.4 crystallizes in the monoclinic space groupC2/c witha=12.062(4),b=21.175(6),c=21.596(5) Å, and β=100.78(4)o withD c =1.18 g cm−3 forZ=4. Refinement based on 2529 observed reflections gaveR=0.082. The Al-O lengths in all three complexes are normal for donor-acceptor interactions.
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  • 4
    ISSN: 1573-1111
    Keywords: Calix[4]arene ; crystal structure ; clay mineral ; alkali metal ion ; layered structure ; water soluble ; sulfonate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title calixarenes all exist in the solid state as bilayers of anionic calixarenes in the cone configuration. These layers alternate with inorganic regions which contain the cations and the water molecules. The overall structures bear a close resemblance to those found for clay minerals. The sodium salt crystallizes in the triclinic space groupPĪ witha = 10.998(6),b = 13.582(5),c = 14.472(5) Å,α = 74.01(3),β = 89.09(4),γ = 86.50(4)°, andZ = 2 forD calc = 1.72 g cm−3. Refinement based on 4727 observed reflections led to a conventionalR = 0.050. The potassium salt crystallizes in the triclinic space groupPĪ witha = 11.815(9),b = 13.636(6),c = 14.040(9) Å,α = 100.24(5),β = 111.86(9),γ = 95,14(9)°, andZ = 2 forD calc = 1.77 g cm−3. Refinement based on 2977 observed reflections led toR = 0.15. The rubidium and cesium salts are isostructural and crystallize in the monoclinic space groupP21/n with parameters for Rb[Cs]a = 11.603(5) [11.704(3)],b = 28.607(8) [29.747(9)],c = 12.512(5) [12.604(4)] Å,β = 91.70(4) [91.63(2)°], andZ = 4 forD calc = 2.01 [2.24] g cm−3. Refinement based on 1750 [4257] observed reflections led toR = 0.108 [0.075]. Disorder of the cations was observed for the rubidium and cesium salts.
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