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Electrochemical one‐electron reduction of dioxomolybdenum complexes with tetradentate N2O2 or N2S2 ligands containing sec. amino groups result in deprotonation of the amino groups and loss of an oxo ligand as H2O. This biomimetically undesirable result is circumvented by synthesis of the ligand (VI) and its complexes (VIII) (which can be prepared also from dioxobis(acetylacetonato)molybdenum and (VI) with 80% yield) and (X).

Outstation, Hamburg, FRG) for measuring the EXAFS spectra.Registry No. [L4Fe4(M-0)2(M-OH)4]I4-3H20, 123567-48-6; [L4Fe4-(µ-0)2(µ-0 )4]( 04)4•3 20, 123567-50-0; [L2Fe2(acac)2^-0)]-(C104)2, 118486-84-3; LFeClj, 86823-88-3. Supplementary Material Available; Tables of complete crystallographic data, bond distances and angles, and thermal parameters (5 pages); a listing of structure factor amplitudes (43 pages). Ordering information is given on any current masthead page.

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