Synthesis and Structural Characterization of ... - Jacobs University

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Chapter 5 Unpublished Results Anderson-Evans type molybdotellurate(VI) has been reported by Bo et al. The same research group also reported the cerium derivative one. 6 A series of lanthanide polyoxomolybdates was synthesized before by the Krebs group by reaction of lanthanide cations with the Anderson-Evans type anion [TeMo 6 O 24 ] 6– . 7 On the other hand, we recently reported two tungstotellurate(IV) anions [H 2 Te 4 W 20 O 80 ] 22− and [NaTeW 15 O 54 ] 13− . 8 2− The two polyanions were synthesized by the reaction of WO 4 and Te 4+ in aqueous medium (pH 7.5). The polyanion [H 2 Te 4 W 20 O 80 ] 22− comprises two {HTe 2 W 10 O 40 } fragments, connected through Te−O−W -oxo bridges, and each containing a pair of face-shared WO 6 octahedra. The polyanion [NaTeW 15 O 54 ] 13− is composed of a triangular assembly of 15 edge- and corner-shared WO 6 octahedra, surrounding a trigonalpyramidal tellurium(IV) center located in the central cavity and a capping sodium ion. The complete lack of molybdotellurates(IV) as such [H 2 Te 4 W 20 O 80 ] 22− and [NaTeW 15 O 54 ] 13− analogues provides an impetus to try to prepare such species. Herein we report on a novel chiral molybdotellurate(IV) structure. 5.A.2.2. Synthesis Na 34 [H 2 Te 24 Mo 44 O 198 ]·84H 2 O (Na-28) A sample of 5.0 g of Na 2 MoO 4·2H 2 O (20.7 mmol) was dissolved in 20 mL H 2 O, followed by dropwise addition of a solution of 0.66 g of TeO 2 (4.1 mmol) in 2 mL concentrated HCl. Then the pH was adjusted to 6.5 using 6M aqueous NaOH. The mixture was vigorously stirred at room temperature for 1 hour, and then filtered. The filtrate was kept in an open vial for crystallization at room temperature. Colorless crystals of Na-28 were obtained after three days which were in turn filtered off and air-dried. Yield: 1.18 g (53.6 %). IR for Na-28 in cm -1 (only between 400-1000 cm -1 ): 925(m), 867(s), 849(s), 808(m), 772(s), 705(m), 667(s), 185
Chapter 5 Unpublished Results 610(m), 569(m), 503(m), 432(m), 407(m) (see Figure 5.9). Anal. Calcd (%) for Na-28: Na, 6.1; Mo, 33.1; Te, 24.2. Found (%): Na, 6.3; Mo, 33.2; Te, 24.3. Figure 5.9. IR spectrum of the compound Na-28. 5.A.2.3. 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. Direct methods (SHELXS97) solutions successfully located the W atoms, and successive Fourier syntheses (SHELXL97) revealed the remaining atoms. 10 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 (Mo, Te) were refined 186
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