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笼中铁：通过四重交联固定Fe(II)tpy配合物

Iron in a Cage: Fixation of a Fe(II)tpy Complex by Fourfold Interlinking.

作者信息

Brandl Thomas, Johannsen Sven, Häussinger Daniel, Suryadevara Nithin, Prescimone Alessandro, Bernhard Stefan, Gruber Manuel, Ruben Mario, Berndt Richard, Mayor Marcel

机构信息

Department of Chemistry, University of Basel, St. Johanns-Ring 19, 4056, Basel, Switzerland.

Institut für Experimentelle und Angewandte Physik, Christian-Albrechts-Universität zu Kiel, Leibnizstr. 19, 24098, Kiel, Germany.

出版信息

Angew Chem Int Ed Engl. 2020 Sep 7;59(37):15947-15952. doi: 10.1002/anie.202006340. Epub 2020 Jun 29.

DOI:10.1002/anie.202006340
PMID:32412664
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC7540000/
Abstract

The coordination sphere of the Fe(II) terpyridine complex 1 is rigidified by fourfold interlinking of both terpyridine ligands. Profiting from an octa-aldehyde precursor complex, the ideal dimensions of the interlinking structures are determined by reversible Schiff-base formation, before irreversible Wittig olefination provided the rigidified complex. Reversed-phase HPLC enables the isolation of the all-trans isomer of the Fe(II) terpyridine complex 1, which is fully characterized. While temperature independent low-spin states were recorded with superconducting quantum interference device (SQUID) measurements for both, the open precursor 8 and the interlinked complex 1, evidence of the increased rigidity of the ligand sphere in 1 was provided by proton T relaxation NMR experiments. The ligand sphere fixation in the macrocyclized complex 1 even reaches a level resisting substantial deformation upon deposition on an Au(111) surface, as demonstrated by its pristine form in a low temperature ultra-high vacuum scanning tunneling microscope experiment.

摘要

Fe(II) 三联吡啶配合物1的配位球通过两个三联吡啶配体的四重交联而刚性化。受益于八醛前体配合物，在不可逆的维蒂希烯烃化反应生成刚性化配合物之前，通过可逆的席夫碱形成确定了交联结构的理想尺寸。反相高效液相色谱法能够分离出Fe(II) 三联吡啶配合物1的全反式异构体，并对其进行了全面表征。虽然通过超导量子干涉装置 (SQUID) 测量记录了开放前体8和交联配合物1的与温度无关的低自旋态，但质子T弛豫核磁共振实验提供了配合物1中配体球刚性增加的证据。大环化配合物1中的配体球固定甚至达到了在沉积在Au(111) 表面时能抵抗大量变形的程度，低温超高真空扫描隧道显微镜实验中的原始形态证明了这一点。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/aa357b5ed105/ANIE-59-15947-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/ac4de4e6cfb6/ANIE-59-15947-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/550d33bdb2c0/ANIE-59-15947-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/73ad92dafd57/ANIE-59-15947-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/901a062e76f2/ANIE-59-15947-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/8156cfafc305/ANIE-59-15947-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/aa357b5ed105/ANIE-59-15947-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/ac4de4e6cfb6/ANIE-59-15947-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/550d33bdb2c0/ANIE-59-15947-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/73ad92dafd57/ANIE-59-15947-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/901a062e76f2/ANIE-59-15947-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/8156cfafc305/ANIE-59-15947-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/052e/7540000/aa357b5ed105/ANIE-59-15947-g005.jpg

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