SYNTHESIS, PROPERTIES AND STRUCTURE OF TRIS(ETHYLNITROSOLATO) COMPLEXES OF MANGANESE, IRON, AND COBALT

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Abstract
A number of complexes derived from ethylnitrosolate (noted L−) have been prepared. Complexes of general formulas ML3 (M=Co, Fe), M ' [ML3] (M=Co, Fe, Mn; M′=N(n [sbnd] C4H9)4, P(C6 H5)4 and MPrime;[ML3] · H2O (M=Fe; M″=Rb, Cs) have been isolated. All the complexes have been characterized by IR, visible and UV spectra measurements, magnetic susceptibility and electrochemical measurements. The voltammetric behaviour shows the existence of three members series of general type ML3 n- (M=Co, Fe, Mn; n=0, 1, 2). All the solids are low-spin. Infrared data support the assumption of the same coordination structure for all the complexes. Some assignments in the IR spectra have been proposed. The crystal structure of Cs[FeL3] · H2O has been determined by single-crystal X-ray diffraction techniques using a full-matrix anisotropic least-squares program (R=0.081). Crystals are monoclinic in the space group P21 / c with cell parameters a=14.97 ± 0.01 Å, b=14.07 ± 0.01 Å, c=14.05 ± 0.01 Å, β=94.31 ± 0.04°. The asymmetric unit consists of two independent molecules. The ligand is bound to the iron atom via the nitrogen atom of the nitroso group and the oxygen atom of the oxime group; the complex has the facial geometry. The average Fe [sbnd] N and Fe [sbnd] O distances are 1.865 and 1.923 Å.