PMID- 25677371 OWN - NLM STAT- MEDLINE DCOM- 20151202 LR - 20171116 IS - 1521-3765 (Electronic) IS - 0947-6539 (Linking) VI - 21 IP - 12 DP - 2015 Mar 16 TI - Tris-functionalized hybrid Anderson polyoxometalates: synthesis, characterization, hydrolytic stability and inversion of protein surface charge. PG - 4762-71 LID - 10.1002/chem.201405644 [doi] AB - 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)3CCH2OH]x12 H2O (1) (TBA = tetrabutylammonium), Na3[FeMo6O18(OCH2)3CCH2OH2]x11 H2O (2), [TMA]2[GaMo6O18(OH)3(OCH2)3CNH3]x7 H2O (3) (TMA = tetramethylammonium), and Na[TMA]2[FeMo6O18(OH)3(OCH2)3CNH3](OH)x6 H2O (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)3CCH2OH]xn H2O (5) and [GDM]3[GaMo6O18(OH)3(OCH2)3CCH2OH]xn H2O (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 degrees 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 mM for compounds 1 and 2, which have the highest negative surface charge. CI - (c) 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. FAU - Blazevic, Amir AU - Blazevic A AD - Institut fur Biophysikalische Chemie, Fakultat fur Chemie, Universitat Wien, Althanstrasse 14, 1090 Wien (Austria). FAU - Al-Sayed, Emir AU - Al-Sayed E FAU - Roller, Alexander AU - Roller A FAU - Giester, Gerald AU - Giester G FAU - Rompel, Annette AU - Rompel A LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20150210 PL - Germany TA - Chemistry JT - Chemistry (Weinheim an der Bergstrasse, Germany) JID - 9513783 RN - 0 (Tungsten Compounds) RN - 0 (polyoxometalate I) RN - 27432CM55Q (Serum Albumin, Bovine) SB - IM MH - Animals MH - Cattle MH - Crystallography, X-Ray MH - Hydrolysis MH - Magnetic Resonance Spectroscopy MH - Molecular Conformation MH - Serum Albumin, Bovine/*chemistry MH - Spectrometry, Mass, Electrospray Ionization MH - Thermogravimetry MH - Tungsten Compounds/chemical synthesis/*chemistry MH - X-Ray Absorption Spectroscopy OTO - NOTNLM OT - POM-protein interactions OT - crystal growth OT - organic-inorganic hybrid composites OT - polyoxometalates EDAT- 2015/02/14 06:00 MHDA- 2015/12/15 06:00 CRDT- 2015/02/14 06:00 PHST- 2014/10/14 00:00 [received] PHST- 2015/02/14 06:00 [entrez] PHST- 2015/02/14 06:00 [pubmed] PHST- 2015/12/15 06:00 [medline] AID - 10.1002/chem.201405644 [doi] PST - ppublish SO - Chemistry. 2015 Mar 16;21(12):4762-71. doi: 10.1002/chem.201405644. Epub 2015 Feb 10.