Organisation profile

Description of the NMR laboratory The High Resolution NMR Centre is basically the NMR lab of the VUB providing all NMR spectra and NMR know how to any researcher of the VUB - or outside the institution - needing NMR for purposes of chemical substance identification and structure determination, either in scientific collaboration, or in service context. This means that, in particular, other research units of the VUB (ORGC, FYSC, FCOL, ULTR, MEMC) make use of these know-how and services on a regular basis. The NMR Centre has profiled itself since 1990 in the advanced chemical structure determination by multinuclear 1D and 2D NMR methods, including its dynamic aspects. The specific own research field of the HNMR team focuses on structural issues on organotin chemistry, addressed by advanced 1D and 2D gradient pulse assisted NMR techniques based on the 119/117Sn nucleus. For the last four years, the scientific interest of the group has evolved towards grafting organotins to soluble and insoluble polymers, aiming at developing applications in the fields of catalysis in transesterification reactions and of potentiometric anion recognition. In this context, numerous external academic joint ventures have been started and are still active with several research teams in Italy, France, Greece, Germany, and several other countries for other projects (see CV R. Willem). Likewise, this novel field of interest has generated interest for the use of NMR at the heterogeneous solid-liquid interface, specifically high resolution Magic Angle Spinning NMR and Diffusion Ordered Spectroscopy. Over the last ten years, HNMR has also been involved in research on organotin compounds with potential antitumour activity. This area of interest has led to different patents, in collaboration with Dr. Dick de Vos of the Dutch company Pharmachemie and Prof. M. Gielen (VUB - POSC). The HNMR group has acknowledged an important equipment grant from the Flemish Science Foundation (Fund for Scientific Research Flanders, FWO) at the beginning of 2002, enabling the lab to apply optimally the above NMR spectroscopic techniques. Students are welcome for Master-theses, and PhD- theses, as are also post-doc researchers for scientific stays of typically one year (financed by e. g. Fund for Scientific Research Flanders, Belgium, FWO, European Marie Curie funding, etc....). The 1D and 2D NMR measurements are performed by the permanent staff members cited above with assistance of the research PhD and Post-Doc researchers. hr-MAS NMR, as well as DOSY NMR measurements are the object of a close collaboration with Prof. Dr. José C. MARTINS, former post-doc researcher of HNMR and presently associate professor (ZAP-hoofddocent) at the University of Ghent; this collaboration also involves the team of Prof. Dr. Guy LIPPENS, with whom the first hr-MAS NMR measurements on samples of the HNMR team have been performed and further collaboration is agreed on. While it is correct to state that the core of the HNMR team is small, and actually has always been, this has not prevented the HNMR team to produce more than 150 internationally peer- reviewed publications over the last ten years, including two reviews, and to present on a regular basis the HNMR team's results at international conferences, as testified by more than 100 congress communications as posters or oral presentations, our during invited lectures. Synthesis laboratory The HNMR team has available a synthesis lab equipped with all the glassware and instrumentation necessary for both standard synthesis and handling air and moisture sensitive organometallic substances (vacuum equipment), completed by an FT-IR spectrometer of the Bruker Biospin company. Apart from the NMR equipment described below, all other organic chemistry analysis tools (GC, MS, LC,...) are available at the laboratory of the ORGC research group (Prof. Dr. Dirk TOURWÉ, Faculty of Sciences), a fine organic synthesis laboratory with which HNMR is collaborating on a regular basis. In this way, the HNMR and ORGC laboratories have a sound, complementary and integrated equipment for performing organic and organometallic synthesis. The HNMR team has had a long tradition of collaboration with Prof. Dr. Marcel GIELEN in the area of structural organotin chemistry. It is the purpose that the HNMR team continues this tradition of organotin synthesis at the VUB, and, in particular, develops further the above- mentioned novel centres of interest around interface and polymer-grafted organotin chemistry. Prof. Dr. Marcel GIELEN has an extended activity as Scientific Editor of Scientific Chemistry Journals Instruments, hardware and software - AMX 500 instrument equipped with: three channels for triple resonance experiments; gradient pulse facilities; triple 5 mm probe 1H-15N-13C with z-gradient coil; multinuclear 5 mm triple probe 1H-dual 119Sn/31P-broad band with z-gradient coil. dedicated triple high resolution Magic Angle Spinning 5 mm probe 1H-13C-119Sn with z- gradient coil; digital lock, high performant preamplifiers, fully linear 1H and X transmitters - AVANCE DRX 250 instrument, equipped with: sample changer and automation routine; triple channel and gradient facilities; solid state CP-MAS facility; Quattro 5 mm probe 1H-13C-19F-117Sn with automatic X- nucleus switch and z-gradient coil; multinuclear 5 mm triple probe 1H-117Sn-broad band (BB) from 109Ag up to 31P with z- gradient coil; BB 10 mm probe, all nuclei at resonance frequencies from 109Ag up to 31P; 1H-BB 7 mm CP-MAS probe with max. 7 KHz spinning rate from 109Ag up to 31P; 1H-BB 4 mm CP-MAS probe with max. 15 KHz spinning rate from 109Ag up to 31P; 19F-BB 4 mm CP-MAS probe with max. 15 KHz spinning rate from 109Ag up to 31P. - Network of computers consisting of two Silicon Graphics O2 R5000 computers, operating respectively the AMX500 and DRX250 spectrometers; two Silicon Graphics Octane R10000 computers for data processing and molecular modelling; one Silicon Graphics Indigo2 computer for data processing and molecular modelling; three PC's for personal routine and more advanced NMR data processing, including one for spectrometer control; straightforward access to all Internet facilities; A4/A3/A0 network accessible printer/plotters on site. - Software package including the basic WIN NMR for acquisition and processing of the data; ACCELRYS software for Life Sciences, INSIGHT 4, DISCOVER, BIOPOLYMER ANALYSIS, DECIPHER; software for NMR data processing and interpretations, FELIX ND, FELIXMODEL, FELIX ASSIGN; software for NMR based structure determination, NMRCHITECT, and a package developed in the group of Prof. K. Wüthrich, ETH Zürich, Switserland, DYANA, NOAH, MOLMOL; TRIPOS software for conformational analysis of small peptides; WIN-DAISY, PERCH, g-NMR for advanced spectrum simulations, including chemical exchange; WIN-MAS, software for solid state spectra simulations. Expertise and Research Topics The High Resolution NMR Centre has expertise and experience in following fields of interest : - advanced structural and conformational characterizations of bio-organic and organotin molecules by multinuclear 2D proton detected heteronuclear correlation techniques; - metabolite analysis in carbon-13 enriched biological extracts by 13C NMR in fundamental diabetology research; - structure characterization of organic polymers; - advanced structural NMR-characterization of organometallic compounds, especially in organotin chemistry, in various applications; -structural analysis of peptides or pseudopeptides, and other organic derivatives with pharmaceutical potential by 2D 1H homonuclear NMR techniques; -applications of organotin chemistry in material and polymer science, using organotins either as precursors to mixed organic-inorganic materials or as functionalities anchored to polymeric materials, either insoluble or soluble intended for applications as anion sensors or catalysts. - liquid and solid state NMR in material sciences. In all these areas of interest, HNMR offers know how focusing on homonuclear 2D NMR (MQF-COSY, E.COSY, TOCSY), including water suppression (e. g. WATERGATE) and gradient pulsed techniques, as well as 3D NMR; 1D and 2D, gradient pulsed, proton detected correlation NMR with heteronuclei, involving carbon-13, phosphorus-31 or low abundant spin-1/2 metal nuclei, mainly tin-119 (or -117); double heteronuclear correlation experiments (carbon13/fluorine-19; fluorine-19/tin-117; phosphorus-31/tin-119, carbon-13/tin- 117/119); all NOESY based applications, homonuclear (NOESY, ROESY, off- res-ROESY) as well as heteronuclear (HOESY); CP-MAS and MAS solid state techniques with carbon-13 and metal nuclei, e.g. silicon-29, aluminum-27, tin-117; 2D exchange spectroscopy, also with low abundant nuclei; in collaboration with Prof. Dr. J. C. Martins, availability of 3D 15N edited NOESY-HSQC and TOCSY-HSQC and their sensitivity enhanced versions, 15N J-HMQC, 13C HSQC, HNCA, HN(CO)CA, HNCO and HN(CA)CO, dedicated to structure analysis of single 15N and double 15N/13C isotopically enriched proteins; advanced theoretical and experimental investigations of 1H- 119(117)Sn J-HMQC and HMBC spectroscopy. diffusion ordered (DOSY) spectroscopy techniques. Collaborations The High Resolution NMR Centre has a well established tradition of collaborations and is open to any proposal of collaboration in any application field of high resolution NMR, with academic as well as industrial partners. It provides measuring time and scientific advise in all kind of NMR applications listed above for all research groups of the VUB needing NMR in their research activity. More information - on the R & D data bank of the VUB : - simply by contacting the staff, in particular for access to NMR instrumentation and expertise, see addresses above. - on the web site of HNMR:

Contact information

Pleinlaan 2
  • Fax: +32-2-6293291
  • Phone: +32-2-6293282

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