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首页> 外文期刊>Chemistry: A European journal >Tris-Functionalized Hybrid Anderson Polyoxometalates: Synthesis, Characterization, Hydrolytic Stability and Inversion of Protein Surface Charge
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Tris-Functionalized Hybrid Anderson Polyoxometalates: Synthesis, Characterization, Hydrolytic Stability and Inversion of Protein Surface Charge

机译：Tris功能化杂化的Anderson多金属氧酸盐：蛋白质表面电荷的合成，表征，水解稳定性和反转

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摘要

Single- and double-sided functionalized hybrid organic-inorganic Anderson polyoxomolybdates with Ga-III 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](3)[GaMo6O18(OH)(3){(OCH2)(3)CCH2OH}]x12H(2)O (1) (TBA=tetrabutylammonium), Na-3[FeMo6O18{(OCH2)(3)CCH2OH}(2)]x11H(2)O (2), [TMA](2)[GaMo6O18(OH)(3){(OCH2)(3)CNH3}]x7H(2)O (3) (TMA=tetramethylammonium), and Na[TMA](2)[FeMo6O18(OH)(3){(OCH2)(3)CNH3}](OH)x6H(2)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](3)[GaMo6O18(OH)(3){(OCH2)(3)CCH2OH}]xnH(2)O (5) and [GDM](3)[GaMo6O18(OH)(3){(OCH2)(3)CCH2OH}]xnH(2)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 100equivalents of 1 or 4 over more than four days at 20 degrees C. Zeta potential measurements demonstrate that 1-4 induce charge inversions on the positively charged surface of BSA (1mgmL(-1)) with concentrations starting as low as 1.29mM for compounds 1 and 2, which have the highest negative surface charge.
机译：Ga-III和Fe-III定位为中心杂原子的单面和双面功能化杂化有机-无机安德森聚氧钼酸酯已在水性介质中以温和的两步合成法合成。分离化合物1-4为水合盐，[TBA]（3）[GaMo6O18（OH）（3）{（OCH2）（3）CCH2OH}] x12H（2）O（1）（TBA =四丁基铵），Na- 3 [FeMo6O18 {（OCH2）（3）CCH2OH}（2）] x11H（2）O（2），[TMA]（2）[GaMo6O18（OH）（3）{（OCH2）（3）CNH3}] x7H （2）O（3）（TMA =四甲基铵）和Na [TMA]（2）[FeMo6O18（OH）（3）{（OCH2）（3）CNH3}]（OH）x6H（2）O（4） 。基于单晶X射线衍射（SXRD），FTIR，UV / Vis，热重分析，ESI-MS，NMR和元素分析对所有化合物进行了表征。化合物1也用两个较小的有机阳离子结晶，得到[TMA]（3）[GaMo6O18（OH）（3）{（OCH2）（3）CCH2OH}] xnH（2）O（5）和[GDM]（3 ）[GaMo6O18（OH）（3）{（OCH2）（3）CCH2OH}] xnH（2）O（6）（GDM =胍），并基于UV / Vis，NMR，FTIR和元素分析进行​​了表征。通过使用ESI-MS在4至9的pH范围内检查其水解稳定性，研究了这些化合物在大分子晶体学中的用途。十二烷基硫酸钠-聚丙烯酰胺凝胶电泳（SDS-PAGE）分析表明，BSA仍保持完整在20摄氏度下超过四天的时间里最多包含100个当量的1或4的溶液。Zeta电势测量表明1-4诱导BSA带正电的表面（1mgmL（-1））上的电荷反转，且浓度从低开始化合物1和2的负表面电荷最高，为1.29mM。

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