Synthesis and Structural Characterization of ... - Jacobs University

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Chapter 5 Published Results K 22 [Co(H 2 O) 2 {Co 3 (B-β-GeW 9 O 33 (OH))(B-β-GeW 8 O 30 (OH))} 2 ]·52H 2 O (K-30) The synthetic procedure was identical to that of K-29, but 0.07 g of CoCl 2·6H 2 O (0.28 mmol) was used instead of CuCl 2·2H 2 O. Slow evaporation of the solvent at room temperature for two weeks resulted in dark-purple crystals. These crystals were isolated and air dried (yield 0.07 g, 13 %). IR for K-30: 941 (m), 889 (m), 867 (m), 841 (m), 812 (sh), 789 (s), 764 (s), 696 (s), 506 (w), 449 (w) cm -1 (see Figure 5.14). Anal. Calcd (%) for K-30: K, 7.9; W, 57.5; Co, 3.8; Ge, 2.7. Found (%): K, 7.0; W, 56.9; Co, 3.5; Ge, 2.5. K 22 [Mn(H 2 O) 2 {Mn 3 (H 2 O)(B-β-GeW 9 O 33 (OH))(B-β-GeW 8 O 30 (OH))} 2 ]·45H 2 O (K-31) The synthetic procedure was identical to K-29, but 0.06 g of MnCl 2·4H 2 O (0.28 mmol) was used instead of CuCl 2·2H 2 O. Slow evaporation of the solvent at room temperature for one day resulted in yellow crystals. These crystals were isolated and air dried (yield 0.08 g, 19 %). IR for K-31: 940 (m), 870 (m), 852 (m), 805 (sh), 789 (s), 764 (s), 706 (m), 520 (w), 494 (w), 449 (w) cm -1 (see Figure 5.14) Anal. Calcd for K-31: K, 8.0; W, 58.1; Mn, 3.6; Ge, 2.7. Found (%): K, 7.1; W, 57.3; Mn, 3.8; Ge, 2.4. Figure 5.14. IR spectra of K-29 (black curve), K-30 (blue curve) and K-31 (green curve) measured on KBr pellets. 201
Chapter 5 Published Results 5.B.3. X‐ray Crystallography Crystals were mounted on a Hampton cryoloop in light oil for data collection at -100 °C. Indexing and data collection were performed on a Bruker D8 SMART APEX II CCD diffractometer with kappa geometry and Mo K radiation (graphite monochromator, = 0.71073 Å). Data integration was performed using SAINT. 29 Routine Lorentz and polarization corrections were applied. Multiscan absorption corrections were performed using SADABS. 30 Direct methods (SHELXS97) successfully located the tungsten atoms, and successive Fourier syntheses (SHELXL97) revealed the remaining atoms. 30 Refinements were full-matrix leastsquares against F 2 using all data. In the final refinement, all non-disordered heavy atoms were refined anisotropically; oxygen atoms and disordered cations were refined isotropically. No hydrogen atoms were included in the models. Crystallographic data are summarized in Table 5.6. Table 5.6. Crystal Data and Structure for K-29, K-30 and K-31. K-29 K-30 K-31 202
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