CRYSTAL AND MOLECULAR-STRUCTURES OF PARA-(1,1,3,3-TETRAMETHYLBUTYL)CALIX[5]ARENE AND ITS 1-1 COMPLEX WITH TOLUENE

A cyclic pentamer was obtained from p-(1,1,3,3-tetramethylbutyl) phenol. It crystallizes from a mixture of acetone and toluene at room temperature giving a 1:1 complex with toluene (compound A), whereas at 50-degrees-C the empty form (compound B) is obtained. Crystals of A are orthorhombic, space group Pna2I, a = 20.083(2), b = 12.936(6), c = 28,423(1) angstrom, Z = 4, final R value = 0.067. The empty form, B, is monoclinic P2(1)/c, a = 18.695(2), b = 11.673(5), c = 35.100(4) angstrom, beta = 114.33(1), Z = 4, final R value = 0.135. The macrocycle is in the cone conformation for both compounds; the toluene molecule lies in the cone as often found for calix[4]arenes.