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Blazevic, Amir
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article
Tris-Functionalized Hybrid Anderson Polyoxometalates: Synthesis, Characterization, Hydrolytic Stability and Inversion of Protein Surface Charge
Abstract
<p>Single- and double-sided functionalized hybrid organic-inorganic Anderson polyoxomolybdates with GaIII and Fe III positioned as central heteroatoms have been synthesized in a mild, two-step synthesis in an aqueous medium. Compounds 1-4 were isolated as hydrated salts, [TBA]<sub>3</sub>[GaMo<sub>6</sub>O<sub>18</sub>(OH)<sub>3</sub>{(OCH<sub>2</sub>)<sub>3</sub>CCH<sub>2</sub>OH}]12H<sub>2</sub>O (1) (TBA= tetrabutylammonium), Na<sub>3</sub>[FeMo<sub>6</sub>O<sub>18</sub>{(OCH<sub>2</sub>)<sub>3</sub>CCH<sub>2</sub>OH}<sub>2</sub>] × 11H<sub>2</sub>O (2), [TMA]<sub>2</sub>[GaMo<sub>6</sub>O<sub>18</sub>(OH)<sub>3</sub>{(OCH<sub>2</sub>)<sub>3</sub>CNH<sub>3</sub>}] × 7H<sub>2</sub>O (3) (TMA = tetramethylammonium), and Na[TMA]<sub>2</sub>[FeMo<sub>6</sub>O<sub>18</sub>-(OH)<sub>3</sub>{(OCH2)<sub>23</sub>CNH}](OH)&times 6H<sub>2</sub>O (4). All the compounds were characterized based on single-crystal X-ray diffraction (SXRD), FTIR, UV/Vis, thermogravimetric, ESI-MS, NMR, and elemental analyses. Compound 1 was also crystallized with two smaller organic cations, giving [TMA]<sub>3</sub>[GaMo<sub>6</sub>O<sub>183</sub>(OH)-{(OCH2)<sub>2</sub>)<sub>3</sub>CCH2OH}] &times n H<sub>2</sub>O (5) and [GDM]<sub>3</sub>[GaMo6O<sub>183</sub>(OH)-{(OCH2)<sub>23</sub>CCH2OH}] &times n H<sub>2</sub>O (6) (GDM = guanidinium) and were characterized based on UV/Vis, NMR, FTIR, and elemental analyses. The use of these compounds as additives in macromolecular crystallography was investigated by examining their hydrolytic stability by using ESI-MS in a pH range of 4 to 9. Sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) analysis showed that BSA remains intact in a solution containing up to 100 equivalents of 1 or 4 over more than four days at 20 8C. Zeta potential measurements demonstrate that 1-4 induce charge inversions on the positively charged surface of BSA (1 mgmL -1) with concentrations starting as low as 1.29 mm for compounds 1 and 2, which have the highest negative surface charge.</p>