Synthesis and Structural Characterization of ... - Jacobs University

Chapter 3
Unpublished Results
Figure 3.36. 89 Y-NMR of Na-17 dissolved in H 2 O/ D 2 O.
3.B.2.5. Conclusions
The mono- and di-lanthanide(III) tungstoantimonates(III) [Ln(H 2 O) 3 Sb 2 W 21 O 72 (OH))] 10− (Ln
= Yb (15), Lu(16), Y(17)) and [Ln 2 (H 2 O) 6 Sb 2 W 20 O 70 )] 8− (Ln = Yb (18), Lu(19), Y(20)) have
been structurally characterized in the solid state by IR spectroscopy, single-crystal XRD,
TGA and elemental analyses. Polyanions 15–20 were synthesized in simple, one-pot reactions
of Ln 3+
ions with the trilacunary polyanion precursor SbW 9 or the Sb 2 W 22 precursor.
Polyanions 15–20 crystallize as sodium salts in the triclinic system, space group P1̅. The
structure of 15–17 comprises the Sb 2 W 20 fragment with one incorporated Ln 3+ ion, whereas
two ions of 18–20. Different synthetic strategies were needed to deliberately and selectively
prepare mono- and di-lanthanide derivatives of Sb 2 W 20 . In this context it was the pH a crucial
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