The first report of the crystal structure of non-solvated μ-oxo boron subphthalocyanine and the crystal structures of two solvated forms.

IF 1.9 3区化学

Acta Crystallographica Section B-structural Science Pub Date : 2012-12-01 Epub Date: 2012-11-16 DOI:10.1107/S0108768112037184

Mabel V Fulford, Alan John Lough, Timothy P Bender

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引用次数: 14

Abstract

The first instance of the solvent-free X-ray determined single-crystal structure of the oxygen-bridged boron subphthalocyanine dimer [μ-oxo-(BsubPc)(2), C(48)H(24)B(2)N(12)O] is reported. Single crystals obtained by train sublimation were found to have μ-oxo-(BsubPc)(2) organized into a C2/c space group. The crystal structure obtained by sublimation is of particular interest as it is highly symmetric and also of notably high density when compared with other BsubPc crystals. The acquisition of this crystal structure came about from the direct chemical synthesis of μ-oxo-(BsubPc)(2) followed by a work-up which culminated in obtaining the single crystals by sublimation. Several methods for the direct chemical synthesis of μ-oxo-(BsubPc)(2) were also investigated each using dichlorobenzene as the solvent. On standing, these reaction mixtures produced a crystal of the dichlorobenzene (DCB) solvate of μ-oxo-(BsubPc)(2) [μ-oxo-(BsubPc)(2)·2DCB]. It is also reported that the conversion of bromo-boron subphthalocyanine (Br-BsubPc) to μ-oxo-(BsubPc)(2) happens on train sublimation which resulted in the acquisition of a partially hydrated crystal [μ-oxo-(BsubPc)(2)·0.25H(2)O].

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首次报道了非溶剂化μ-氧硼亚酞菁的晶体结构及两种溶剂化形式的晶体结构。

报道了首次用无溶剂x射线测定氧桥硼亚酞菁二聚体[μ-氧-(BsubPc)(2)， C(48)H(24)B(2)N(12)O]的单晶结构。通过列升华得到的单晶中，μ-oxo-(BsubPc)(2)组成C2/c空间群。通过升华获得的晶体结构是特别有趣的，因为它是高度对称的，而且与其他BsubPc晶体相比，密度也很高。这种晶体结构的获得是通过μ-氧-(BsubPc)(2)的直接化学合成，然后通过升华最终获得单晶。研究了以二氯苯为溶剂直接化学合成μ-氧-(BsubPc)(2)的几种方法。在静止状态下，这些反应混合物产生μ-氧-(BsubPc)(2) [μ-氧-(BsubPc)(2)·2DCB]的二氯苯(DCB)溶剂晶体。也有报道称，溴-硼亚酞菁(Br-BsubPc)在列升华过程中转化为μ-氧-(BsubPc)(2)，得到部分水合晶体[μ-氧-(BsubPc)(2)·0.25H(2)O]。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Acta Crystallographica Section B-structural Science 化学-晶体学

自引率

5.30%

发文量

审稿时长

6-12 weeks

期刊介绍： Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials publishes scientific articles related to the structural science of compounds and materials in the widest sense. Knowledge of the arrangements of atoms, including their temporal variations and dependencies on temperature and pressure, is often the key to understanding physical and chemical phenomena and is crucial for the design of new materials and supramolecular devices. Acta Crystallographica B is the forum for the publication of such contributions. Scientific developments based on experimental studies as well as those based on theoretical approaches, including crystal-structure prediction, structure-property relations and the use of databases of crystal structures, are published.