Synthesis, solid-state structure, magnetic properties and Mössbauer spectral studies of {Fe[HC(3,5-Me2pz)3](H2O)3}(BF4)2

✍ Scribed by Daniel L. Reger*; Christine A. Little; Arnold L. Rheingold; Roger Sommer; Gary J. Long*

• Publisher: Elsevier Science
• Year: 2001
• Tongue: English
• Weight: 133 KB
• Volume: 316
• Category: Article
• ISSN: 0020-1693
• DOI: 10.1016/s0020-1693(01)00381-4

✦ Synopsis

The reaction of Fe(BF 4 ) 2 •6H 2 O and one equivalent of HC(3,5-Me 2 pz) 3 in acetonitrile leads to the formation of {Fe[HC(3,5-Me 2 pz) 3 ](H 2 O) 3 }(BF 4 ) 2 . The solution phase 1 H NMR spectrum is broad with chemical shifts ranging from 54 to -42 ppm, a range that is indicative of a paramagnetic high-spin complex. Magnetic moment measurements show that the complex is paramagnetic in the solid-state with v eff =4.89v B . The solid-state structure shows the N 3 FeO 3 central core is a distorted octahedron with N-Fe-N angles averaging 84.4°and O -Fe-O angles averaging 90.0°. The average Fe-N distance is 2.18 A , and the average Fe-O bond distance is 2.12 A , . Mo ¨ssbauer spectra, obtained at 78 and 295 K, clearly reveal that this complex is high-spin at these temperatures with hyperfine parameters typical of a pseudooctahedral iron(II) complex.