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Chapter 5 Published Results 5.A.1.2. Synthesis Na 22 [H 2 Te 4 W 20 O 80 ]·64H 2 O (Na-26) A sample of 10.00 g of Na 2 WO 4·2H 2 O (30.3 mmol) was dissolved in 20 mL 1M NaCl, followed by dropwise addition of a solution of 1.07 g of TeO 2 (6.7 mmol) in 2.5 mL concentrated HCl. Then the pH was adjusted to 7.5 using 4M aqueous HCl, and a white sticky precipitate was formed. The mixture was vigorously stirred at room temperature for 1 h, and then the precipitate was filtered off and discarded. The filtrate was kept in an open vial for crystallization at room temperature. After a day, colorless crystals of paradodecatungstate ([H 2 W 12 O 42 ] 10- ) started to appear and were filtered off successively and discarded until needle-shaped, colorless crystals of Na-26 were formed (after ~1 week). These crystals were in turn filtered off and air-dried. Yield: 0.77 g (7.1 %). IR for Na-26 in cm -1 (only between 400-1000 cm -1 ): 925(m), 873(m), 848(w), 801(sh), 738(s), 692(m), 619(w), 475(w), 421(w), see Figure 5.1. Figure 5.1. IR spectrum of Na 22 [H 2 Te 4 W 20 O 80 ]·64H 2 O (Na-26). 167
Chapter 5 Published Results 5.A.1.3. X‐ray Crystallography All crystals were mounted in Hampton cryoloops using light oil, for data collection at low temperature. Indexing and data collection were performed using a Bruker X8 APEX II CCD diffractometer with kappa geometry and Mo K α radiation (λ = 0.71073 Å). Data integration and routine processing were performed using the SAINT software suite. Further data processing, including multi-scans absorption corrections, was performed using SADABS. 13 Direct methods (SHELXS97) solutions successfully located the W atoms, and successive Fourier syntheses (SHELXL97) revealed the remaining atoms. 13 Refinements were fullmatrix least squares against F 2 using all data. Some cations and waters of hydration were modeled with varying degrees of occupancy, a common situation for polyoxotungstate structures. In the final refinements, all nondisordered heavy atoms (W, Te) were refined anisotropically, while the O and Na atoms were refined isotropically. No H atoms were included in the models. The crystallographic data are provided in Table 5.1. Selected bond lengths and angles are listed in Table 5.2 and Table 5.3, respectively. 168
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