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100K下环四(μ-5,10,15,20-四-4-吡啶基卟啉)四锌(II)二甲基甲酰胺八水合物三水合物的重新测定

Redetermination of cyclo-tetra-kis-(μ-5,10,15,20-tetra-4-pyridyl-porphyrinato)tetra-zinc(II) dimethyl-formamide octa-solvate trihydrate at 100 K.

作者信息

Seidel Rüdiger W, Graf Jürgen, Goddard Richard, Oppel Iris M

出版信息

Acta Crystallogr Sect E Struct Rep Online. 2011 Jan 22;67(Pt 2):m236-7. doi: 10.1107/S1600536811002054.

Abstract

The structure of the title compound, [Zn(4)(C(40)H(24)N(8))(4)]·8C(3)H(7)NO·3H(2)O, has been redetermined at 100 K. The redetermination is of significantly higher precision and gives further insight into the disorder of pyridyl groups and solvent mol-ecules. The mol-ecules of (5,10,15,20-tetra-4-pyridyl-porphyrinato)zinc(II) (ZnTPyP) form homomolecular cyclic tetra-mers by coordination of a peripheral pyridyl group to the central Zn atom of an adjacent symmetry-related mol-ecule. The tetra-mer so formed exhibits mol-ecular S(4) symmetry and is located about a crystallographic fourfold rotoinversion axis. Severely disordered dimethyl-formamide and water mol-ecules are present in the crystal, the contributions of which were omitted from refinement. Inter-molecular C-H⋯N hydrogen bonding is observed.

摘要

标题化合物[Zn₄(C₄₀H₂₄N₈)₄]·8C₃H₇NO·3H₂O的结构已在100 K下重新测定。此次重新测定具有显著更高的精度,并对吡啶基和溶剂分子的无序性有了进一步的了解。(5,10,15,20-四-4-吡啶基-卟啉锌(II))(ZnTPyP)分子通过一个外围吡啶基与相邻对称相关分子的中心Zn原子配位形成同分子环状四聚体。如此形成的四聚体具有分子S₄对称性,且位于一个晶体学四重旋转反演轴上。晶体中存在严重无序的二甲基甲酰胺和水分子,在精修过程中未考虑它们的贡献。观察到分子间的C—H⋯N氢键。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e65c/3051794/f567cc535ab2/e-67-0m236-fig1.jpg

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