Synthesis, Structure, and Characterization of the New [L(OH)Fe(μ-O)Fe(OH2)L]3+ Complex (L = N,N‘-Dimethyl-N,N‘-bis(2-pyridylmethyl)ethane-1,2-diamine). Detection of an Equilibrium with the Protonated Diamond Form [LFe(μ-O)(μ-OH)FeL]3+ in Acetonitrile
| Autor: | Jean Guilhem, Sandrine Poussereau, Geneviève Blondin, Michèle Cesario, Geneviève Chottard, Florence Gonnet, Jean-Jacques Girerd |
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| Rok vydání: | 1998 |
| Předmět: | |
| Zdroj: | Inorganic Chemistry. 37:3127-3132 |
| ISSN: | 1520-510X 0020-1669 |
| DOI: | 10.1021/ic971589e |
| Popis: | The complex [L(H2O)Fe(μ-O)Fe(OH)L](ClO4)3·H2O, where L = N,N‘-dimethyl-N,N‘-bis(2-pyridylmethyl)ethane-1,2-diamine, was synthesized. It crystallizes in the orthorhombic space group P212121 with a = 13.283(5) A, b = 16.050(9) A, c = 20.050(9) A, V = 4476(6) A3, and Z = 4. It presents the hydrogen-bonded [(H2O)Fe(μ-O)Fe(OH)]3+ core unit characterized by an Fe−O−Fe angle of 137.5(2)° and an Fe−Fe distance of 3.396(1) A. The measurement of the magnetic susceptibility as a function of the temperature indicated an antiferromagnetic coupling between the two high-spin Fe(III) ions J = −184 cm-1 (H = −JS1·S2). In the solid state the symmetric stretching vibration was observed at 438 cm-1. Upon dissolution in dry acetonitrile, this vibration was no longer detected and an intense band was observed at 600 cm-1. This frequency can be correlated with an Fe−O−Fe angle of 111°. This value suggests that the species which exists in these conditions is the protonated diamond core [Fe(μ-O)(μ-OH)Fe]3+, analogous to that ident... |
| Databáze: | OpenAIRE |
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