1,4-Bis(4-ferrocenylphenylethynyl)anthraquinone by synchrotron X-ray powder diffraction
1,4-Bis(4-ferrocenylphenylethynyl)anthraquinone by synchrotron X-ray powder diffraction
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1,4-双(4-二茂铁基苯乙炔基)蒽醌同步加速器X射线粉末衍射
DOI：
10.1107/s0108270113013978
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发表时间：
2013
期刊：
影响因子：
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通讯作者：
Hiroshi Nishihara
中科院分区：
文献类型：
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作者：
Maki Sachiko;Eiji Nishibori;Masanori Yoshida;Shinobu Aoyagi;Makoto Sakata;Masaki Takata;Mio Kondo;Masaki Murata;Ryota Sakamoto;Hiroshi Nishihara
合成了标题化合物[Fe2(C5H5)2(C40H22O2)]或1,4-(FcPh)2Aq[其中FcPh为2-（4-二茂铁苯基）乙基，Aq为蒽醌]，试图获得一种新的含溶剂多孔材料，具有较大的空隙空间。热力学数据表明1,4-(FcPh)2Aq在430 K左右发生相变。在90、300和500 K温度下，用同步加速器粉末衍射数据测定了无溶剂的1,4-(FcPh)2Aq的晶体结构。采用遗传算法的直接空间法求解结构。利用最大熵法根据观察到的结构因子计算电荷密度，对模型进行改进。最终模型通过多级Rietveld细化得到。在这两种相中，平面Aq片段以相反的方向交替堆叠，形成一维柱状结构。FcPh臂位于堆叠之间，填充剩余空间，不留下空隙。Ph和Fc片段之间的C-H⋯π相互作用介导晶体堆积和稳定。
The title compound, [Fe2(C5H5)2(C40H22O2)] or 1,4-(FcPh)2Aq [where FcPh is 2-(4-ferrocenylphenyl)ethynyl and Aq is anthraquinone], was synthesized in an attempt to obtain a new solvent-incorporating porous material with a large void space. Thermodynamic data for 1,4-(FcPh)2Aq show a phase transition at approximately 430 K. The crystal structure of solvent-free 1,4-(FcPh)2Aq was determined at temperatures of 90, 300 and 500 K using synchrotron powder diffraction data. A direct-space method using a genetic algorithm was employed for structure solution. Charge densities calculated from observed structure factors by the maximum entropy method were employed for model improvement. The final models were obtained through multistage Rietveld refinements. In both phases, the structures of which differ only subtly, the planar Aq fragments are stacked alternately in opposite orientations, forming a one-dimensional column. The FcPh arms lie between the stacks and fill the remaining space, leaving no voids. C—H⋯π interactions between the Ph and Fc fragments mediate crystal packing and stabilization.