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5,11,17,23-四叔丁基-25,26,27,28-四[2-(2-氯乙氧基)乙氧基]-2,8,14,20-四磺酰基杯[4]芳烃

5,11,17,23-Tetra-tert-butyl-25,26,27,28-tetra-kis[2-(2-chloro-ethoxy)eth-oxy]-2,8,14,20-tetra-sulfonyl-calix[4]arene.

作者信息

Hu Ling, Liu Yang, Ma Jiang-Ping, Guo Dian-Shun

机构信息

Department of Chemistry, Shandong Normal University, Jinan 250014, People's Republic of China.

出版信息

Acta Crystallogr Sect E Struct Rep Online. 2009 Jan 28;65(Pt 2):o385-6. doi: 10.1107/S1600536809002591.

Abstract

Mol-ecules of the title compound, C(56)H(76)Cl(4)O(16)S(4), have crystallographic C(2) symmetry and adopt a 1,3-alternate conformation where the four -OCH(2)CH(2)OCH(2)CH(2)Cl groups are located alternately above and below the virtual plane (R) defined by the four bridging S atoms. The dihedral angles between the plane (R) and the phenolic rings are 72.85 (7) and 74.57 (7)°. An unusual 24-membered macrocyclic ring is formed in the crystal structure with an array of eight intra-molecular C-H⋯O hydrogen bonds between the ether arm H atoms and the sulfonyl O atoms. In the supra-molecular structure, the mol-ecular components are linked into infinite zigzag one-dimensional chains by a combination of four inter-molecular C-H⋯O hydrogen bonds, forming R(2) (2)(13), R(2) (2)(16), R(2) (2)(21) and R(2) (2)(26) ring motifs. These chains are augmented into a wave-like two-dimensional network by weak C⋯O inter-actions. One tert-butyl group shows rotational disorder, and one CH(2)CH(2)Cl group is disordered over two orientations; the site-occupation factors are 0.756 (6) and 0.244 (6) for the two tert-butyl groups, and 0.808 (3) and 0.192 (3) for the two CH(2)CH(2)Cl units.

摘要

标题化合物C(56)H(76)Cl(4)O(16)S(4)的分子具有晶体学C(2)对称性,呈1,3-交替构象,其中四个-OCH(2)CH(2)OCH(2)CH(2)Cl基团交替位于由四个桥连S原子定义的虚拟平面(R)的上方和下方。平面(R)与酚环之间的二面角为72.85 (7)°和74.57 (7)°。晶体结构中形成了一个不寻常的24元大环,醚臂H原子与磺酰基O原子之间存在一系列八个分子内C-H⋯O氢键。在超分子结构中,分子组分通过四个分子间C-H⋯O氢键的组合连接成无限之字形一维链,形成R(2) (2)(13)、R(2) (2)(16)、R(2) (2)(21)和R(2) (2)(26)环基序。这些链通过弱C⋯O相互作用扩展成波浪状二维网络。一个叔丁基表现出旋转无序,一个CH(2)CH(2)Cl基团在两个取向上无序;两个叔丁基的占位因子分别为0.756 (6)和0.244 (6),两个CH(2)CH(2)Cl单元的占位因子分别为0.808 (3)和0.192 (3)。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5471/2968348/9a5306389cd3/e-65-0o385-fig1.jpg

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