Crystal structures of two calix[10]arenes complexed with neutral molecules

Two calix[10]arenes were synthesized: the tert-butyl calix[10]arene (t-Bu-C 10) and the detertbutylated analogue (H-C10). Both were crystallized from s aturated solutions: t-Bu-C10 from a mixture of toluene and tetrahydrofuran (THF), H-C10 from acetone. In each case, complexes were obtained: H-C10, ac etone 1:2 and t-Bu-C10, toluene, THF 1:2.5:0.5. The crystal structures of t hese two complexes and the different conformations of the macrocycles are p resented here. For the first, the crystals are triclinic, space group Pmacr {1}, a = 9.037(2)Angstrom, b = 11.447(2)Angstrom, c = 15.197(3)Angstrom, al pha = 80.79(3)Angstrom, beta = 84.96(3)degrees, gamma = 88.60(3)degrees, V = 1545.7(5)Angstrom (3), Z = 1; the complex with t-Bu-C10 is orthorhombic, space group Fmm2, a = 32.211(6)Angstrom, b = 32.289(7)Angstrom, c = 12.179( 2)Angstrom, V = 12667(4)Angstrom (3), Z = 4. The complex from H-C10 shows a pleated loop conformation with H-bonds between acetone and hydroxyl groups . The complex from t-Bu-C10 shows several cavities, in the cones shaped by the phenol moieties and near the hydroxyl groups. The packings are given fo r both crystals.