Tetrahomodioxa p-phenylcalix(4)arene dihexylether (C66H68O6)를 합성하여 분자 및 결정 구조를 X-선 회절법으로 연구하였다. p-Phenylphenol의 탈수, 고리화 반응으로 만든 tetrahomodioxa p-phenylcalix(4)arene을 DMF에서 NaH와 hexyl iodide를 환류시켜 합성하였다. 결정은 사방정계이고 공간군은 P2₁2₁2₁, a =9.764(2), b = 16.167(2), c = 32.994(3) Å, V=5208(1) ų, Z= 4, Dc=1.221 gcm-3이다. 직접법으로 구조를 해석하였으며, 최소자승법으로 정밀화하여 최종 신뢰도 R 값은 2009개의 회절 반점에 대해 0.070 이었다. 이 분자는 마주 보고 있는 phenyl group 두 쌍이 거의 평행을 이루며, C-1,2-alternate conformation이고, lower rim의 1,3 위치에 hexyl 기가 치환된 비대칭 homooxacalixarene이다.
Tetrahomodioxa p-phenylcalix(4)arene dihexylether(C66H68O6) has been synthesized and structurally characterized by X-ray diffraction. Reaction of tetrahomodioxa p-phenylcalix(4)arene with hexyl halide and NaH in DMF leads to the dihexyl derivatives, 7,13,21,27-tetraphenyl-29,31-dihexyloxy- 2,3,16,17-tetrahomo-3,17-dioxacalit(4)arenes. The crystal is orthorhombic, P2₁2₁2₁, a= 9.764(2), b=16.167(2), c=32.994(3) Å, V=5208(1) Å, Z= 4, Dc = 1.221 gcm-3. The structure was solved by direct methods and refined by full-matrix least squares. Refinement converged at R = 0.070 for 2009 observed reflections. This molecule has a C-1,2-alternate conformation with pseudo-centrosymmetry and has two pairs of opposite phenyl rings, which are approximately parallel to each other. The benzene rings A and B are up, and the rings C and D rings are down with respect to the plane of the macrocyclic ring.
