Synthesis and Structural Characterization of ... - Jacobs University
Synthesis and Structural Characterization of ... - Jacobs University
Synthesis and Structural Characterization of ... - Jacobs University
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Chapter 3<br />
Unpublished Results<br />
K 8 Cs 3 Na[(Lu(GeW 11 O 39 )(H 2 O)) 2 (-CH 3 COO) 2 ]·18H 2 O (KCsNa-23)<br />
The same procedure as KCsNa-21 was followed, except for using 0.067 g LuCl 3·6 H 2 O <strong>and</strong><br />
adding <strong>of</strong> 0.5 mL <strong>of</strong> 0.5M CsCl (aq) to the filtrate. Yield: 0.763 g (55 %). IR data for KCs-23:<br />
1625(m), 1530(m), 1459(m), 1397(w), 1351(sh), 950(s), 893(s), 809(s), 779(sh), 746(w),<br />
678(s), 615(sh), 526(m), 497(sh), 466(m), 446(w) cm -1 (see Figure 3.37). Anal. Calcd for<br />
KCsNa-23: K, 4.5; Na, 0.33; Cs, 5.6; Ge, 2.1; W, 57.5; Lu, 5.1; C, 0.69; H, 0.72. Found: K,<br />
4.5; Na, 0.1; Cs, 5.2; Ge, 2.1; W, 60.2; Lu, 5.1; C, 0.75; H, 0.73.<br />
For the compounds K-21 – KCsNa-23, the b<strong>and</strong>s in the range from 1000 – 400 cm -1 represent<br />
the fingerprint region <strong>of</strong> the polyoxometalate lig<strong>and</strong>, while the region from 1351 – 1530 cm -1<br />
correspond to the acetate lig<strong>and</strong>s bridged to the metal centers (Figure 3.37). 1a,4<br />
Elemental analyses were carried out by Zentralabteilung für chemische Analysen,<br />
Forschungszentrum Jülich GmbH, Jülich, Germany.<br />
Figure 3.37. IR spectra <strong>of</strong> the K-21 (blue line), K-22 (balck line), <strong>and</strong> KCsNa-23 (red line)<br />
(from bottom to top).<br />
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