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Iron in a Cage: Fixation of a Fe(II)tpy2 Complex by Fourfold Interlinking.

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 T2 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.

SUBMITTER: Brandl T 

PROVIDER: S-EPMC7540000 | biostudies-literature | 2020 Sep

REPOSITORIES: biostudies-literature

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Iron in a Cage: Fixation of a Fe(II)tpy<sub>2</sub> Complex by Fourfold Interlinking.

Brandl Thomas T   Johannsen Sven S   Häussinger Daniel D   Suryadevara Nithin N   Prescimone Alessandro A   Bernhard Stefan S   Gruber Manuel M   Ruben Mario M   Berndt Richard R   Mayor Marcel M  

Angewandte Chemie (International ed. in English) 20200629 37

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 temper  ...[more]

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