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  • X-ray crystal structure  (5)
  • Springer  (5)
  • 1
    ISSN: 1573-1111
    Keywords: Dicyclohexano-24-crown-8 ; hydronium uranyl chloride methanol solvate complex ; hydronium uranium(IV) chloride methanol solvate complex ; X-ray crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The reaction of dicyclohexano-24-crown-8 with UCl4 in 3/1 THF:MeOH under anhydrous conditions and with exposure to air, resulted in the isolation of the hydronium ion complexes, [(H5O2)(dicyclohexano-24-crown-8)]2[UO2Cl4]-MeOH and [(H5O2)(dicyclohexano-24-crown-8)]2[UCI6]-MeOH. The [UO2Cl4]2− complex crystallizes in the monoclinic space group,P21/n, witha = 15.200(8),b = 26.565(9),c = 16.977(8)Å, β = 95.89(6)° andD calc = 1.40 g cm−3 forZ = 4 formula units. A finalR value of 0.051 was obtained utilizing 5913 independent observed [F o ≥ 5σ(F o)] reflections. One ether is complexed by an ordered H5O inf2 sup+ ion, while the second crown ether is hydrogen bonded to a disordered H5O inf2 sup+ ion. The [UCl6]2− complex is tetragonal,P4/n, with (at −150°C)a = 16.320(4),c = 12.542(2)Å andD calc = 1.47 g cm−1 forZ = 2. A finalR value of 0.038 was obtained utilizing 2466 observed reflections. The anion resides on a four-fold axis and the crown ether cation around a crystallographic two-fold axis. The H5O inf2 sup+ ion is disordered into two orientations within the macrocycle cavity. All three crystallographically independent crown ether environments in these two structures have essentially identical conformations.
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  • 2
    ISSN: 1573-1111
    Keywords: Nitrobenzo-15-crown-5 ; dinitrobenzo-15-crown-5 ; dinitrodibenzo-18-crown-6 acetonitrile solvate ; X-ray crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structures of three nitrated benzocrown ethers have been determined. Nitrobenzo-15-crown-5 crystallizes in the orthorhombic space group,Pca21, witha = 15.367(2),b = 4.8499(8),c = 19.963(5)Å, andD calc = 1.40 g cm−3 forZ = 4. Dinitrobenzo-15-crown-5 crystallizes in the monoclinic space group,P21/n, witha = 11.716(2),b = 8.495(3),c = 17.441(5)Å,β = 108.40(2)° andD calc = 1.44 g cm−3 forZ = 4.Dinitrodibenzo-18-crown-6·2CH3CN ismonoclinic,P21/n,witha = 8.138(2),b = 20.435(9),c = 15.953(9)Å,β = 100.55(4)° andD calc = 1.36 g cm−3 forZ = 4. The nitro substituents are in the plane of the benzo ring except in the sterically congested dinitrobenzo-15crown-5. The observed crown ether conformations are similar to their substituted analogs.
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 8 (1990), S. 375-382 
    ISSN: 1573-1111
    Keywords: 12-crown-4 ; cerium nitrate complex ; X-ray crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A unique cerium nitrate complex, [Ce(NO3)3(OH2)(12-crown-4)]-12-crown-4, has been crystallized from the reaction of hydrated cerium nitrate and 12-crown-4. It crystallizes in the orthorhombic space group,Pnma, with (at −150°C)a = 22.901(5),b = 13.547(3),c = 8.422(1)Å, andD x = 1.77 g cm−3 forZ = 4 formula units. A finalR value of 0.048 was obtained utilizing 2059 unique observed [F o ⩾ 5σ(F o)] reflections. The Ce atom resides on a crystallographic mirror plane and is 11-coordinate, coordinated to three bidentate nitrate groups, one water molecule and the four oxygens of one 12-crown-4 molecule. The water molecule hydrogen bonds a second 12-crown-4 unit. Both unique crown molecules and one of the nitrate anions are severely disordered.
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 4 (1986), S. 351-358 
    ISSN: 1573-1111
    Keywords: 12-crown-4 ; yttrium ; complex ; X-ray crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Y(NO3)3(12-crown-4) was prepared via reaction of the crown ether and Y(NO3)3·nH2O in acetonitrile. Y(NO3)3(12-crown-4) crystallizes in the monoclinic space groupP21/c witha=12.084(5),b=8.524(4),c=15.150(6) Å, β=91.62(3)0 andD calc=1.92 g cm−3 forZ=4. The structure was refined by least-squares to a final conventionalR value of 0.105 using 1249 independent observed reflections [I≥3σ(I)]. The title compound is isostructural with its Eu(III) analog. The yttrium ion is ten-coordinate, bonded to three bidentate nitrate groups and to the four oxygens of the crown ether. The coordination polyhedron is best described as a 4A, 6B-extended dodecahedron. The Y-O(nitrate) and Y-O(ether) separations average 2.44(5) and 2.46(4) Å, respectively.
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 15 (1993), S. 145-152 
    ISSN: 1573-1111
    Keywords: 20-thiocrown-4 ; X-ray crystal structure ; crown ether
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An improved synthesis of 20-thiocrown-4 is reported, which exploits the Kellogg method of cesium carbonate in DMF mediated macrocyclization of precondensed synthones which converge at the cycloicosane structure. The crystal structure of 20-thiocrown-4 reveals a rectangular conformation for the free ligand. Each sulfur is in onegauche and oneanti torsion angle. Four carbon positions make up the corners. There are two short sides comprised of −C−C− torsion angle sequencesg −ag− and two long sides (aaa, g −ag+). The S−C and C−C bond distances average 1.816(2) Å and 1.523(3) Å, respectively.
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