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2,25-二氧代-27,28-二苯基-30-氧杂-29-硫杂-3,10,17,24-四氮杂五环-[24.2.1.1.0.0]三十碳-5,7,9(4),10,12,14,16,18,20,22,26,28-十二碳烯氯仿溶剂化物

2,25-Dioxo-27,28-diphenyl-30-oxa-29-thia-3,10,17,24-tetra-aza-penta-cyclo-[24.2.1.1.0.0]triaconta-5,7,9(4),10,12,14,16,18,20,22,26,28-dodeca-ene chloro-form disolvate.

作者信息

Askerov Rizvan K, Roznyatovsky Vladimir V, Katayev Evgeny A, Maharramov Abel M, Khrustalev Victor N

出版信息

Acta Crystallogr Sect E Struct Rep Online. 2010 Feb 20;66(Pt 3):o660-1. doi: 10.1107/S1600536810006173.

Abstract

The macrocycle of the title compound, C(36)H(24)N(4)O(3)S·2CHCl(3), contains a rigid framework with the nitro-gen and oxygen heteroatoms pointing in towards the center of the macrocyclic cavity. The macrocycle is essentially planar (r.m.s. deviation = 0.027 Å) except for the thio-phene ring. The dihedral angle between the thio-phene ring plane and the mean plane of the central macrocyclic core including all atoms except sulfur is 21.6 (1)°. Four intra-molecular hydrogen bonds occur: two are between the amide hydrogen atoms and the Schiff base nitro-gen atoms, while the others are between the amide hydrogen atoms and the sulfur atom of the thio-phene. The two solvate chloro-form mol-ecules are bound to the carbonyl oxygen atoms of the ligand by weak C-H⋯O hydrogen bonding. In addition, the structure reveals inter-molecular Cl⋯Cl close contacts [3.308 (2), 3.404 (2) and 3.280 (2) Å] between the chloro-form solvate mol-ecules. In the crystal, the macrocycles form layers parallel to (101), with an inter-layer distance of 3.362 (3) Å. This short distance is determined by the stacking inter-actions between the amide carbonyl and imine fragments of neighboring ligands.

摘要

标题化合物C(36)H(24)N(4)O(3)S·2CHCl(3)的大环包含一个刚性骨架,其中氮和氧杂原子指向大环腔的中心。除噻吩环外,大环基本呈平面状(均方根偏差 = 0.027 Å)。噻吩环平面与包括除硫之外的所有原子的中心大环核心平均平面之间的二面角为21.6 (1)°。存在四个分子内氢键:两个是酰胺氢原子与席夫碱氮原子之间的氢键,另外两个是酰胺氢原子与噻吩的硫原子之间的氢键。两个溶剂化氯仿分子通过弱C-H⋯O氢键与配体的羰基氧原子相连。此外,该结构揭示了氯仿溶剂化分子之间的分子间Cl⋯Cl紧密接触[3.308 (2)、3.404 (2)和3.280 (2) Å]。在晶体中,大环形成平行于(101)的层,层间距为3.362 (3) Å。这个短距离是由相邻配体的酰胺羰基和亚胺片段之间的堆积相互作用决定的。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/89cd/2983673/a3c0435cd04d/e-66-0o660-fig1.jpg

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