Senge Mathias O., Medforth Craig J., Forsyth Timothy P., Lee David A., Olmstead Marilyn M., Jentzen Walter, Pandey Ravindra K., Shelnutt John A., Smith Kevin M.
Department of Chemistry, University of California, Davis, California 95616, Institut für Organische Chemie (WE02), Freie Universität Berlin, Takustrasse 3, D-14195 Berlin, Germany, and Fuel Science Department, Sandia National Laboratories, Albuquerque, New Mexico 87185-0710.
Inorg Chem. 1997 Mar 12;36(6):1149-1163. doi: 10.1021/ic961156w.
Conformational analysis of highly substituted porphyrins has potential implications for modeling the behavior of macrocycles in tetrapyrrole-containing protein complexes and during catalytic reactions. In order to study the influence of different substituent patterns on the conformation of the porphyrin macrocycle, a series of metal free and nickel(II) decasubstituted porphyrins bearing aryl or ethyl groups at opposite meso positions and alkyl groups at the pyrrole positions have been synthesized and characterized by X-ray crystallography. Crystal structures of the free-base porphyrins with 5,15-diaryl substituents showed negligible out-of-plane distortion but a large amount of in-plane distortion along the 5,15-axis accompanied by large bond angle changes similar to those previously seen for related porphyrins with 5,15-dialkyl substituents. Nickel(II) complexes of the 5,15-diaryl-substituted porphyrins show planar or modestly nonplanar conformations, suggesting that these complexes are not intrinsically nonplanar, whereas a complex with 5,15-diethyl substituents has a very ruffled conformation similar to those observed for related complexes with other metals. The nickel(II) complexes are also elongated along the 5,15-axis in a qualitatively similar but less dramatic fashion than are the free-base porphyrins. Spectrosopic studies ((1)H NMR, optical, and resonance Raman spectroscopy) suggest that conformations similar to those determined by X-ray crystallography are present in solution for the 5,15-dialkyl- and 5,15-diaryl-substituted porphyrins. Several asymmetric nickel(II) and metal-free deca- and undecasubstituted porphyrins containing both aryl and alkyl meso-substituents were also investigated. Metal-free 5,15-disubstituted porphyrins with one aryl and one alkyl group showed considerably elongated porphyrin cores, whereas nickel(II) complexes of porphyrins with 5,10- or 5,10,15-substitution patterns showed very nonplanar structures consisting mainly of ruffle and saddle type distortions.
高度取代卟啉的构象分析对于模拟含四吡咯蛋白复合物中以及催化反应过程中大环的行为具有潜在意义。为了研究不同取代模式对卟啉大环构象的影响,合成了一系列在相对的中位带有芳基或乙基且在吡咯位置带有烷基的无金属和镍(II)十取代卟啉,并通过X射线晶体学对其进行了表征。具有5,15-二芳基取代基的游离碱卟啉的晶体结构显示出可忽略不计的面外扭曲,但沿5,15轴存在大量面内扭曲,并伴有与之前观察到的具有5,15-二烷基取代基的相关卟啉类似的大键角变化。5,15-二芳基取代卟啉的镍(II)配合物呈现平面或适度非平面构象,这表明这些配合物并非本质上非平面,而具有5,15-二乙基取代基的配合物具有非常褶皱的构象,类似于观察到的具有其他金属的相关配合物。镍(II)配合物沿5,15轴也有伸长,其定性方式与游离碱卟啉相似,但程度较小。光谱研究((1)H NMR、光学和共振拉曼光谱)表明,对于5,15-二烷基和5,15-二芳基取代的卟啉,溶液中存在与通过X射线晶体学确定的构象相似的构象。还研究了几种同时含有芳基和烷基中位取代基的不对称镍(II)以及无金属的十取代和十一取代卟啉。具有一个芳基和一个烷基的无金属5,15-二取代卟啉显示出卟啉核显著伸长,而具有5,10-或5,10,15-取代模式的卟啉的镍(II)配合物呈现出非常非平面的结构,主要由褶皱和鞍型扭曲组成。