Abstract
The crystal structures of oxo-centered trineclear cobalt-iron chloroacetate complex [CoIIFe III2 O(CH2ClCO2)6(H2O)3]·3H2O (1) was compared with that of previously reported trinuclear iron complex [FeIIFe III2 O(CH2ClCO2)6(H2O)3]·3H2O (2) which has an isomorphous structure to 1. Compound 1 crystallizes in space group P21/n with Z=4 in a unit cell of a=14.826 (4) Å, b=4.536 (8) Å, c=14.000 (4) Å, β=100.32 (2)0 and V=2968 (11) Å3. The structure was refined to R=0.75 and Rw=0.82. The coordination geometries of the three iron atoms are observed equivalent in 1 indicating a static disorder of the position among cobalt and iron atoms. Two distinct FeIII doublets observed in Mössbauer spectra of 1 become an indistinguishable broad doublet by dehydration of crystal water. On the other hand, no significant line-broadening is observed after the dehydration in complex 2. The results indicate that the dehydration in 2 induces a local environmental change reordering of an electronic configuration around iron atoms, whereas the remaining disordering is reflected in Mössbauer spectrum after the dehydration in 1.
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T. SATO, T. NAKAMOTO, M. KATADA, K. ENDO, H. SANO, Proceedings of the RIKEN Int. Symp., Unstable Nuclei and Particles as Probes in Physics and Chemistry (UN3PC92), RIKEN, 1992, Hyperfine Interactions, 84 (1994) 559. Full manuscript was submitted for publication.
Crystal data for C12H24Cl6CoFe2O19: fw=855.66, monoclinic, space group P21/n (No. 14), a=14.826 (4) Å, b=14.536 (8) Å, c=14.000 (4) Å, β=100.32 (2), V=2968 (11) Å3, Z=4, Dcalcd=1.91 g/cm3, R=7.5%, Rw=8.2%. Crystal data for C12H24Cl6Fe3O19: fw=852.57, monoclinic, space group P21/n (No. 14), a=14.846 (1) Å, b=14.463 (2) Å, c=14.036 (1) Å, β=100.329 (5)0, V=2965.1 (5) Å3, Z=4, Dcalcd=1.91 g/cm3, R=3.4%, Rw=4.0%.
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Sato, T., Ambe, F., Endo, K. et al. Crystal structures and Mössbauer spectroscopic studies of oxo-centered trinuclear chloroacetate complexes. Journal of Radioanalytical and Nuclear Chemistry, Articles 190, 257–261 (1995). https://doi.org/10.1007/BF02040001
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DOI: https://doi.org/10.1007/BF02040001