Synthesis of Double-Bridged Cofacial Nickel Porphyrin Dimers with 2,2'-Bipyridyl Pillars and Their Restricted Coordination Space.,Inorganic Chemistry

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Synthesis of Double-Bridged Cofacial Nickel Porphyrin Dimers with 2,2'-Bipyridyl Pillars and Their Restricted Coordination Space.
Inorganic Chemistry ( IF 4.3 ) Pub Date : 2020-05-22 , DOI: 10.1021/acs.inorgchem.0c00177
Akiharu Satake _{1,

2} , Yuta Katagami ₁ , Yuki Odaka ₁ , Yusuke Kuramochi _{1,

2} , Shohei Harada ₁ , Takaya Kouchi ₁ , Hajime Kamebuchi _{1,

3} , Makoto Tadokoro _{1,

3}

Affiliation

Double-bridged cofacial Ni porphyrin dimers 2 with 2,2′-bipyridyl pillars were effectively prepared by a one-step reductive homocoupling reaction of bis(chloropyridyl)-substituted Ni porphyrin derivatives followed by a specific separation of a cyanopropyl-modified silica gel column using pyridine eluent systems. The structural analyses of 2 and its Pd complex were carried out in their solid and solution states by means of X-ray single crystal analysis and NMR, respectively. The complexation of η³-allylpalladium chloride (Pd) with 2 on the spatially restricted 2,2-bipyridine moieties on 2 gave a 2:1 (Pd:2) complex, in which the 2,2′-bipyridine ligands only provided one of the N atoms on a 2,2′-bipyridine ligand to a Pd. Therefore, the 2,2-bipyridine moieties acted as a monodentate ligand.

中文翻译：

具有2,2'-联吡啶柱的双桥界面镍卟啉二聚体的合成及其受限的配位空间。

通过双（氯吡啶基）取代的镍卟啉衍生物的一步还原均偶联反应，然后通过氰基丙基改性硅胶柱的特定分离，可有效制备具有2,2'-联吡啶基柱的双桥面镍卟啉二聚体2。使用吡啶洗脱液系统。分别通过X射线单晶分析和NMR对2及其Pd配合物进行了固相和固溶状态的结构分析。的η络合³ π-烯丙基氯（钯）与2上的空间受限的2,2-联吡啶基部分上2给了一个2：1（钯：2）配合物，其中2,2'-联吡啶配体仅向Pd提供2,2'-联吡啶配体上的N原子之一。因此，2，2-联吡啶部分起单齿配体的作用。

更新日期：2020-05-22

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