| Title | Unprecedented oxo-titanium citrate complex precipitated from aqueous citrate solutions, exhibiting a novel bilayered Ti8O10 structural core |
| Publication Type | Journal Article |
| Year of Publication | 2004 |
| Authors | Kemmitt, T., Al-Salim N.I., Gainsford G.J., Bubendorfer A., and Waterland M. |
| Journal | Inorganic Chemistry |
| Volume | 43 |
| Issue | 20 |
| Pagination | 6300 - 6306 |
| Date Published | 2004 |
| ISSN | 00201669 (ISSN) |
| Keywords | aqueous solution, article, carbon nuclear magnetic resonance, carboxylic acid, Chelation, Citrates, citric acid, crystal structure, Crystallization, Crystallography, X-Ray, microscopy, Models, Molecular, Organometallic Compounds, oxotitanium citrate, powder, precipitation, Solutions, Spectrum Analysis, Raman, structure analysis, Titanium, titanium 2 propoxide, titanium derivative, titanium dioxide, unclassified drug, water, X ray analysis |
| Abstract | Aqueous titanium citrate solutions were prepared from the reaction of citric acid with titanium 2-propoxide in a range of molar ratios. Solutions containing two or fewer citrates per titanium resulted in the slow crystallization of an insoluble titanium oxo-citrate complex. Single-crystal X-ray analysis identified the species as Ti8O10(citrate) 4-(H2O)12·14H2O· 3HOPri, crystallized in the tetragonal space group I41/a, with a = 30.775(7) Å, c = 14.528(7) Å, V = 13759(8) Å3, and Z= 8. The trianionic citrate ligands supply both carboxylate and alkoxide coordination and stabilize the structure using simultaneous chelating and bridging modes of attachment. The compound is a neutral species, exhibiting titanium in three contrasting environments. Laser Raman microscopy and 13C CPMAS solid-state NMR data were consistent with those of the X-ray crystal structure. When exposed to air, the crystals rapidly lost water and became a powder. The dehydrated powder was noncrystalline to X-rays and insoluble, but 13C NMR results demonstrated retention of the carboxylate linkages. |
| URL | http://www.scopus.com/inward/record.url?eid=2-s2.0-4644286231&partnerID=40&md5=88c0e84d3cd27687ec0d2111e49539a0 |
| DOI | 10.1021/ic049760r |
