Cosublimation: A Rapid Route Toward Otherwise Inaccessible Halogen-Bonded Architectures
Cosublimation: A Rapid Route Toward Otherwise Inaccessible Halogen-Bonded Architectures
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DOI：
10.1021/acs.cgd.8b01089
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发表时间：
2018-08
影响因子：
3.8
通讯作者：
Patrick M. J. Szell;S. Gabriel;Estelle Caron‐Poulin;O. Jeannin;M. Fourmigué;D. L. Bryce
中科院分区：
文献类型：
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作者：
Patrick M. J. Szell;S. Gabriel;Estelle Caron‐Poulin;O. Jeannin;M. Fourmigué;D. L. Bryce
有几种合成技术可用于制备卤素键合加合物，包括传统的溶剂蒸发方法和机械化学。为了减少溶剂用量和实验次数，我们建立了共升华法制备卤素键合共晶，重点研究含氮杂环的C-I···N基序。我们选择了四种常见的卤素键供体（I2，1，4-二碘苯，1，4-二碘四氟苯，1，3，5-三氟-2，4，6-三碘苯）和四个卤素键受体（2，3，5，6-四甲基吡嗪，1，4-二氮杂双环[2.2.2]辛烷，2，2 ′-联吡啶，1-金刚烷腈），由于它们的挥发性范围，并通过以下方法探索了所有16种组合：溶剂蒸发、使用双区炉在密封玻璃管中过夜共升华和在真空升华装置中加速共升华。我们表明，从过夜共升华获得的粗晶体是合适的质量的。
Several synthetic techniques are available for the preparation of halogen-bonded adducts, including traditional solvent-evaporation methods and mechanochemistry. With the intention of reducing solvent usage and experimental times, we establish cosublimation as a synthetic technique for preparing halogen-bonded cocrystals, focusing on the C–I···N motif involving nitrogen-containing heterocycles. We selected four common halogen-bond donors (I2, 1,4-diiodobenzene, 1,4-diiodotetrafluorobenzene, 1,3,5-trifluoro-2,4,6-triiodobenzene) and four halogen-bond acceptors (2,3,5,6-tetramethylpyrazine, 1,4-diazabicyclo[2.2.2]octane, 2,2′-bipyridyl, 1-adamantanecarbonitrile), by virtue of their range in volatility, and explored all 16 combinations via the following methods: solvent evaporation, overnight cosublimation in a sealed glass tube using a two-zone furnace, and expedited cosublimation in a vacuum sublimation apparatus. We show that the raw crystals obtained from overnight cosublimation are of suitable quality f...