Synthesis, Characterization, and Crystal Structure of a (μ-Oxo)bis(μ-acetato)diiron(III) Complex with a Dinucleating Hexapyridine Ligand, 1,2-Bis[2-(bis(2-pyridyl)methyl)-6-pyridyl]ethane. the First Example of a Discrete (μ-Oxo)bis(μ-acetato)diiron(III) Complex with a Dinucleating Ligand

Masahito Kodera, Hisashi Shimakoshi, Masato Nishimura, Hisashi Okawa, Seiichiro Iijima, Koji Kano

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Abstract

A mononucleating tripyridine ligand, 2-(bis(2-pyridyl)methyl)-6-methylpyridine (L1), and a dinucleating hexapyridine ligand, 1,2-bis[2-(bis(2-pyridyl)methyl)-6-pyridyl]ethane (L2), have been prepared. The reaction of a carbanion of 2,6-lutidine with 2-bromopyridine affords L1 which is converted to L2 quantitatively by treating with tert-butyllithium and 1,2-dibromoethane. (μ-Oxo)bis(μ-acetato)diiron(III) complexes [Fe2(O)(OAc)2(L1)2]-(ClO 4)2 (1) and [Fe2(O)(OAc)2L2](ClO4)2 (2) have been synthesized and characterized by means of infrared, UV/vis, mass, and Mössbauer spectroscopies and by measuring magnetic susceptibility and cyclic voltammograms. All the spectral data are consistent with the (μ-oxo)bis(μ-acetato)diiron(III) core structure in both 1 and 2. A relatively strong molecular ion peak at m/z 865 corresponding to [{Fe2O(OAc)2L2}(ClO4)]+ in a FAB mass spectrum of 2 suggests the stabilization of the (μ-oxo)bis(μ-acetato)diiron(III) core structure by L2 in a solution state. The compound 2·DMF·2-PrOH·H2O, chemical formula C44Cl2Fe2H51N7O 16, crystallizes in the monoclinic space group C2/c with a = 22.034(6) Å, b = 12.595(5) Å, c = 20.651(7) Å, β= 121.49(2)°, and Z = 4. The cation has 2-fold symmetry with the bridging oxygen atom on the 2-fold axis: Fe-(μ-O) = 1.782(5) Å, Fe-O-Fe = 123.6(6)°, and Fe⋯Fe = 3.142(3) Å. The diiron(III) core structure of 2 seems to be stabilized by encapsulation of the ligand. Compound 2 is the first example of a discrete (μ-oxo)bis(μ-acetato)diiron(III) complex with a dinucleating ligand.

Original languageEnglish
Pages (from-to)4967-4973
Number of pages7
JournalInorganic chemistry
Volume35
Issue number17
DOIs
Publication statusPublished - Jan 1 1996
Externally publishedYes

All Science Journal Classification (ASJC) codes

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

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