Synthesis and Structural Characterization of ... - Jacobs University

Chapter 3
Unpublished Results
Anal. Calcd for Na-15: Na, 3.5; Sb, 3.7; W, 59.7; Yb, 2.7. Found: Na, 3.2; Sb, 3.7; W, 59.0;
Yb, 2.8.
Na 10 [Lu(H 2 O) 3 Sb 2 W 21 O 72 (OH)]·42H 2 O (Na-16)
The same procedure as Na-15 was followed, except for using 0.068 g LuCl 3·6H 2 O. Yield:
0.022 g (4 %). IR data for Na-16: 953(s), 874(sh), 840(m), 806(s), 758(m), 660(m), 525(w),
517(w), 472(w), 459(w), 431(w), 417(w) cm -1 (see Figure 3.27). Anal. Calcd for Na-16: Na,
3.5; Sb, 3.8; W, 59.5; Lu, 2.7. Found: Na, 3.2; Sb, 3.8; W, 58.7; Lu, 3.2.
Na 10 [Y(H 2 O) 3 Sb 2 W 21 O 72 (OH)]·40H 2 O (Na-17)
The same procedure as Na-15 was followed, except for using 0.044 g YCl 3·6H 2 O. Yield:
0.033 g (6 %). IR data for Na-17: 953(s), 874(sh), 840(m), 806(s), 758(m), 660(m), 525(w),
517(w), 472(w), 459(w), 431(w), 417(w) cm -1 (see also Figure 3.27). Anal. Calcd for Na-17:
Na, 3.6; Sb, 3.8; W, 60.6; Y, 1.4. Found: Na, 3.2; Sb, 3.8; W, 59.1; Y, 1.4.
Using Sb 2 W 22 precursor:
Na 10 [Yb(H 2 O) 3 Sb 2 W 21 O 72 (OH)]·41H 2 O (Na-15)
0.031 g (0.079 mmol) of YbCl 3·6H 2 O was added to 20 mL 1M NaCl (aq) with stirring followed
by addition of 0.50 g (0.079 mmol) of Na 12 [Sb 2 W 22 O 74 (OH) 2 ], and then the pH was adjusted
to 5 with 1M NaOH. The solution was stirred at 50 ˚C for 30 min, allowed to cool to room
temperature. The filtrate was kept in an open vial for crystallization. After about one week
colorless crystals were obtained, which were filtered off and air dried (yield 0.40 g, 79 %). IR
for Na-15 showed metal-oxygen stretches at 953(s), 874(sh), 840(m), 806(s), 758(m), 660(m),
525(w), 517(w), 472(w), 459(w), 431(w), 417(w) cm -1 (see Figure 3.27). Anal. Calcd for Na-
15: Na, 3.5; Sb, 3.7; W, 59.7; Yb, 2.7. Found: Na, 3.2; Sb, 3.7; W, 59.0; Yb, 2.8.
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