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Iron(III) complexes with 2‐pyridyl oxime ligands: Synthesis, structural and spectroscopic characterization, and magnetic studies
Author(s) -
Tzani Sofia,
Lazarou Kateri.,
Stoumpos Constantinos C.,
Pissas Michael,
Psycharis Vassilis,
Sanakis Yiannis,
Raptopoulou Catherine P.
Publication year - 2016
Publication title -
chemistryselect
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.437
H-Index - 34
ISSN - 2365-6549
DOI - 10.1002/slct.201600037
Subject(s) - chemistry , oxime , zwitterion , electron paramagnetic resonance , picolinic acid , stereochemistry , medicinal chemistry , magnetic susceptibility , crystallography , molecule , nuclear magnetic resonance , organic chemistry , physics
Reactions of Fe III sources with 2‐pyridyl oxime ligands, pyC(R)NOH (R=H, Me, Ph), afforded the trinuclear oxo‐centered complexes (NH 4 )[Fe 3 O(LH) 6 (H 2 O) 3 ](ClO 4 ) 8 ⋅MeOH⋅1.14H 2 O ( 1 ⋅ MeOH⋅1.14H 2 O) and [Fe 3 O{pyC(H)NO)(PhCO 2 ) 6 (H 2 O)]⋅MeCN ( 2 ⋅MeCN), the tetranuclear complex [Fe 4 (OH) 4 {pyC(Me)NO} 4 (H 2 O) 4 ] (ClO 4 ) 4 ⋅3Me 2 CO⋅H 2 O ( 3 ⋅3Me 2 CO⋅H 2 O), and the hexanuclear complexes [Fe 6 (OH) 6 {pyC(Me)NO} 6 (H 2 O) 6 ](ClO 4 ) 6 ⋅8Me 2 CO⋅2H 2 O ( 4 ⋅8Me 2 CO⋅2H 2 O), [Fe 6 (OH) 6 {pyC(Me)NO} 6 (MeCONH 2 ) 6 ](ClO 4 ) 6 ⋅2MeCN⋅H 2 O ( 5 ⋅2MeCN⋅H 2 O), [Fe 6 (OH) 6 {pyC(Ph)NO} 6 (H 2 O) 6 ](ClO 4 ) 6 ⋅4.4Me 2 CO ⋅1.6Et 2 O ( 6 ⋅4.4Me 2 CO ⋅1.6Et 2 O) and [Fe 6 (OH) 6 {pyC(Ph)NO} 6 (MeOH) 6 ](ClO 4 ) 5.5 (OH) 0.5 ⋅MeOH⋅0.5H 2 O ( 7 ⋅MeOH ⋅0.5H 2 O), where LH is the zwitterion anionic form of 2‐pyridinecarboxylic acid (picolinic acid). Complex 3 can be described as inverse 12‐metallacrown‐4, whereas 4–7 can be described as inverse 18‐metallacrowns‐6 and represent the first examples of iron(III) metallacyclic clusters with pyC(R)NOH (R=H, Me, Ph) ligands. Complexes 3 and 6 were characterized by Mössbauer spectroscopy and magnetic susceptibility measurements, while complex 2 was characterized by EPR spectroscopy.