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Chapter 3 Unpublished Results Anal.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. 117
Chapter 3 Unpublished Results Na 10 [Lu(H 2 O) 3 Sb 2 W 21 O 72 (OH)]·42H 2 O (Na-16) The same procedure as Na-15 was followed, except for using 0.031 g LuCl 3·6H 2 O. Yield: 0.38 g, 75 %. 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 0.020 g YCl 3·6H 2 O. Yield: 0.35 g (70 %). 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. Figure 3.27. IR spectra of the three compounds Na-15 (blue curve), Na-16 (green curve), and Na-17 (balck curve) (from bottom to top). 118
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