四甲基铵
化学
水解
核化学
水溶液
傅里叶变换红外光谱
热重分析
溶剂分解
有机化学
离子
量子力学
物理
作者
Amir Blazevic,Emir Al‐Sayed,Alexander Roller,Gerald Giester,Annette Rompel
标识
DOI:10.1002/chem.201405644
摘要
Abstract 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 [GaMo 6 O 18 (OH) 3 {(OCH 2 ) 3 CCH 2 OH}]×12 H 2 O ( 1 ) (TBA=tetrabutylammonium), Na 3 [FeMo 6 O 18 {(OCH 2 ) 3 CCH 2 OH} 2 ]×11 H 2 O ( 2 ), [TMA] 2 [GaMo 6 O 18 (OH) 3 {(OCH 2 ) 3 CNH 3 }]×7 H 2 O ( 3 ) (TMA=tetramethylammonium), and Na[TMA] 2 [FeMo 6 O 18 (OH) 3 {(OCH 2 ) 3 CNH 3 }](OH)×6 H 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 [GaMo 6 O 18 (OH) 3 {(OCH 2 ) 3 CCH 2 OH}]× n H 2 O ( 5 ) and [GDM] 3 [GaMo 6 O 18 (OH) 3 {(OCH 2 ) 3 CCH 2 OH}]× n H 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 100 equivalents of 1 or 4 over more than four days at 20 °C. Zeta potential measurements demonstrate that 1 – 4 induce charge inversions on the positively charged surface of BSA (1 mg mL −1 ) with concentrations starting as low as 1.29 m M for compounds 1 and 2 , which have the highest negative surface charge.
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