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Chapter 3 Unpublished Results K 8 Cs 3 Na[(Lu(GeW 11 O 39 )(H 2 O)) 2 (-CH 3 COO) 2 ]·18H 2 O (KCsNa-23) The same procedure as KCsNa-21 was followed, except for using 0.067 g LuCl 3·6 H 2 O and adding of 0.5 mL of 0.5M CsCl (aq) to the filtrate. Yield: 0.763 g (55 %). IR data for KCs-23: 1625(m), 1530(m), 1459(m), 1397(w), 1351(sh), 950(s), 893(s), 809(s), 779(sh), 746(w), 678(s), 615(sh), 526(m), 497(sh), 466(m), 446(w) cm -1 (see Figure 3.37). Anal. Calcd for 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, 4.5; Na, 0.1; Cs, 5.2; Ge, 2.1; W, 60.2; Lu, 5.1; C, 0.75; H, 0.73. For the compounds K-21 – KCsNa-23, the bands in the range from 1000 – 400 cm -1 represent the fingerprint region of the polyoxometalate ligand, while the region from 1351 – 1530 cm -1 correspond to the acetate ligands bridged to the metal centers (Figure 3.37). 1a,4 Elemental analyses were carried out by Zentralabteilung für chemische Analysen, Forschungszentrum Jülich GmbH, Jülich, Germany. Figure 3.37. IR spectra of the K-21 (blue line), K-22 (balck line), and KCsNa-23 (red line) (from bottom to top). 137
Chapter 3 Unpublished Results 3.B.3.3. X‐ray Crystallography The crystallographic data are summarized in Table 3.7. Table 3.7. Crystal Data and Structure Refinement for K-22 – KCsNa-23. Code K-22 KCsNa-23 Empirical formula H 50 C 4 Gd 2 Ge 2 O 98 W 22 K 12 H 50 C 4 Lu 2 Ge 2 O 98 W 22 K 12 Cs 3 Na MW 6561.8 8543.0 Crystal system Monoclinic Monoclinic Space group (no.) P2 1 /c P2 1 /c aÅ 19.996(5) 19.793(2) bÅ 12.612(3) 12.5836(12) cÅ 21.047(4) 20.952(2) ° 90 90 ° 110.922(8) 111.983(5) ° 90 90 V/Å 3 4957.7(19) 4839.0(9) Z 2 2 T/ ºC -100 -100 λÅ 0.71073 0.71073 D/ Mg m -3 4.396 5.863 μ/ mm -1 27.85 30.05 R[I >2sigma(I)] a 0.058 0.038 R w (all data) b 0.142 0.121 __________________________ a R = ∑|F o | – |F c | |∑| |F o |. b R w = {∑[w(F o 2 – F c 2 ) 2 ] / ∑[w(F o 2 ) 2 ]} 1/2 . 138
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