Neutral catecholate derivatives of manganese and iron: Synthesis and characterization of the metal-oxygen cubane-like species M sub 4 (DBCat) sub 4 (py) sub 6 (M = Mn, Fe), the trinuclear complex Mn sub 3 (DBCat) sub 4 (py) sub 4 , and the dimers M sub 2 (DBCat) sub 2 (py) sub n (M = Mn, n = 6; M = Fe, n = 4, 6)
- Univ. of California, Davis (United States)
The synthesis and characterization of several new catecholate derivatives of manganese and iron are described. The reaction of 3,5-di-tert-butylcatechol (DBCatH{sub 2}) with the amides M(N(SiMe{sub 3}){sub 2}){sub 2} (M = Mn, Fe) in the presence of pyridine (py) affords the title compounds in high yield. The dimers Mn{sub 2}(DBCat){sub 2}(py){sub 6} (1) and Fe{sub 2}(DBCat){sub 2}(py){sub n} (n = 4 (4a), 6 (4b)) are obtained by treatment of catechol with the appropriate amide in pyridine. In hexane or toluene, this reaction gives the tetrametallic species M{sub 4}(DBCat){sub 4}(py){sub 6} (M = Mn (2), Fe (5)) upon the addition of 2 equiv of pyridine or, in the case of 2, by recrystallization of the dimer from toluene. Mn{sub 3}(DBCat){sub 4}(py){sub 4} (3) is obtained by slow air oxidation of 2 or by addition of 1/3 equiv of 3,5-di-tert-butyl-o-benzoquinone to the reaction of Mn(N(SiMe{sub 3}){sub 2}){sub 2} with DBCatH{sub 2} in hexane with subsequent addition of pyridine. Compounds 1-5 were characterized by infrared, UV-visible, {sup 1}H NMR, and EPR spectroscopy and X-ray crystallography.
- OSTI ID:
- 6967328
- Journal Information:
- Inorganic Chemistry; (United States), Journal Name: Inorganic Chemistry; (United States) Vol. 31:6; ISSN 0020-1669; ISSN INOCA
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
140505* -- Solar Energy Conversion-- Photochemical
Photobiological
& Thermochemical Conversion-- (1980-)
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400500 -- Photochemistry
AMIDES
AROMATICS
AZINES
BOND ANGLE
BOND LENGTHS
CHEMICAL PREPARATION
CHEMICAL REACTION KINETICS
CHEMICAL REACTIONS
COHERENT SCATTERING
COMPLEXES
CRYSTAL LATTICES
CRYSTAL STRUCTURE
DERIVATIZATION
DEVELOPERS
DIFFRACTION
DIMENSIONS
DIMERS
ELECTRON SPIN RESONANCE
ELECTRON TRANSFER
HETEROCYCLIC COMPOUNDS
HYDROXY COMPOUNDS
INFRARED SPECTRA
IRON COMPLEXES
KINETICS
LENGTH
LIGANDS
MAGNETIC RESONANCE
MANGANESE COMPLEXES
NMR SPECTRA
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
OXIDATION
PHENOLS
PHOTOCHEMICAL REACTIONS
POLYPHENOLS
PYRIDINES
PYROCATECHOL
REACTION KINETICS
RECRYSTALLIZATION
RESONANCE
SCATTERING
SPECTRA
SYNTHESIS
TRANSITION ELEMENT COMPLEXES
TRIGONAL LATTICES
ULTRAVIOLET SPECTRA
X-RAY DIFFRACTION