The reaction of ytterbium metal with ammonium tri-fluoro-acetate in liquid ammonia resulted in a green substance comprising a substantial amount of ytterbium(II) tri-fluoro-acetate that is a useful precursor for the oxidative synthesis of the new ytterbium(III) compound, [(NH) (HO) ][YbF(OCCF)(HO)]·4HO ( = 1/4), in aqueous tri-fluoro-acetic acid. This mixed ammonium/oxonium crystalline solid is the first example of a substance containing an -hexa-nuclear ytterbium(III) complex with μ-face-capping fluorido ligands. The main structural features of its [YbF] core are non-bonding Yb⋯Yb distances and Yb-F bond lengths of 3.7576 (3)-3.9413 (5) and 2.2375 (17)-2.3509 (17) Å, respectively. Yb-O bond lengths involving the O atoms of ,'-bridging carboxyl-ato ligands and vertex-substituting aqua ligands are in the ranges 2.23 (4)-2.329 (2) and 2.448 (2)-2.544 (3) Å, respectively. These bond lengths are in accordance with expectations, taking into account lanthanoid contraction. Inter-estingly, there is a significant ammonium oxonium ion site dependence, not only of the hydrate water mol-ecule positions within the solid's hydrogen-bonding framework, but also of the coordination sites of one carboxyl-ato and one aqua ligand in the hexa-nuclear complex.
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| http://dx.doi.org/10.1107/S2056989022004790 | DOI Listing |
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