SMASH 2017 Conference Program
Sunday, September 17th
09:00 - 16:00 Vendor user meetings
- Mestrelab research users' meeting - Registration and Program (external link)
- Bruker BioSpin users' meeting - Registration and Program (external link)
- ACDLabs users' meeting (NOT at the Hotel Dino) - Registration and Program (external link)
17:00 - 18:00 Registration - Grand Hotel Dino
18:00 - 20:00 Mixer - Grand Hotel Dino
20:00 - 22:00 Dinner - Grand Hotel Dino
Monday, September 18th
09:00 - 09:15 Welcome, announcements and opening remarks
09:15 - 10:50 I still haven't found what I'm looking for - New approaches to structure elucidation
Chair: Peter Howe, Syngenta
"The principal current approach to elucidating structures by NMR relies on 1) through-bond connectivities deduced from proton-carbon HMBC and HSQC spectra and proton-proton COSY and TOCSY spectra 2) likely covalent bonding deduced from proton and carbon chemical shifts. These may be supplemented with information from other nuclei, including 19F and 15N. Although extremely powerful, this approach faces difficulties in molecules that contain few protons or fused ring structures because chemical shifts and J-couplings both give ambiguous information. Therefore, the scientific literature still regularly features structural reassignments based on data from total synthesis or X-ray crystallography. This session will consider new experimental and computational approaches to address the current weaknesses of structure elucidation. Possible approaches include: quantitative interpretation of proton-carbon and proton-proton J-couplings; use of the Nuclear Overhauser Effect or dipolar couplings; carbon-carbon correlation methods; improved methods of ranking proposed structures; and combination of NMR with other methods such as MS and HPLC."
Josep Sauri, Merck Sharp & Dohme - Structure Elucidation Group, Boston, USA: Complex Structural Problems and Unconventional NMR Methods to Solve Them
Teo Parella, UAB, Spain: New NMR Methods to Improve the Measurement of One-Bond Proton-Carbon Coupling Constants
Alexei Buevich, Merck Sharp & Dohme - Department of Discovery and Preclinical Sciences, Kenilworth USA: Synergistic Combination of CASE Algorithms and DFT Chemical Shift Predictions for Structure Elucidation, Verification and Revision
Roberto Gil, Department of Chemistry, Carnegie Mellon University, Pittsburgh, PA, USA: Computer-Assisted 3D Structure Elucidation of Small Molecules Using Residual Dipolar Couplings and Isotropic 13C Chemical Shifts (upgraded poster)
10:50 - 11:30 Break
11:30 - 12:30 Workshop 1: Pure and simple - Understanding Pure shift NMR methodology
Chair: Laura Castañar-Acedo, The University of Manchester
"Currently, pure shift NMR is an area of high interest. The aim of this workshop is to cover the practical aspects of these experiments. First, we will briefly describe the different methods available, their implementation in conventional 1D and multidimensional NMR experiments, and we will show several practical applications reported in recent years. The main part of the workshop will then deal with the practical features of pure shift experiments, such as optimal acquisition parameters and post-processing. No NMR experiment is perfect, and pure shift experiments are no exception. Some of the problems/limitations, such as sensitivity and spectral quality, will therefore also be discussed, as well as the techniques available for their removal/reduction. Finally, we will have an open question and answer session about all of the aspects covered, and about the challenges and possible next steps in the amazing adventure of the development and application of pure shift NMR experiments."
12:30 - 14:00 Lunch
14:00 - 15:35 All Shook Up - Metabolites and multi-component samples
Chair: Carla Marchioro, Research 4 Rent (R4R)
"Analytical methodologies and insights for analyses of multi-component samples will be discussed with emphasis on spectroscopic techniques. Chemical and biological mixtures will be covered ranging from identification of metabolites and food components to chemical reactions understanding."
Julien Wist, Chemistry Department, Universidad del Valle, Cali, Colombia: Mutual Diffusion Driven Experiments and Cheminformatics to Demystify Complex Mixtures
Jean-Marc Nuzillard, Institut de Chimie Moléculaire de Reims, CNRS UMR 7312, Reims, France: Complementary Approaches to Mixture Analysis
Carlotta Ciaramelli, University of Milano-Bicocca, Milan, Italy: 1H-NMR to Evaluate the Metabolome of Bronchoalveolar Lavage Fluid (BALf) in Bronchiolitis Obliterans Syndrome (BOS)
Joep van Rijn, DSM Biotechnology Center, Delft, The Netherlands: Robust and Reliable Quantification of Phospholipids in Edible Oils (upgraded poster)
15:35 - 16:00 Break
16:00 - 17:00 Workshop 2: Got to get you into my life - A guide to Solid-state NMR for solution state spectroscopists
Chair: Peter Gierth, Bruker
"Solid state NMR is a tool with a large range of applications to small molecules, including providing spectra of insoluble compounds, polymorphism studies, analysis of solid mixtures, investigation of protonation states. Historically solid-state NMR has been seen as an exotic technique, requiring large amounts of specialised hardware and considerable operator experience, limiting its wider use. In recent years the improvements of general NMR hardware have allowed sophisticated solid state NMR experiments on standard instruments with simple addition of a probe and pneumatic spinning unit, and this combined with an increasing array of relevant experimental techniques has increased interest in solid-state NMR among the general NMR community. This workshop will cover hardware requirements, some basic experimental procedures, and examples of applications of classical and recently developed techniques to small molecule problems."
17:00 - 17:30 Free time
17:30 - 18:30 Shoolery Award Lecture
James Keeler, University of Cambridge, UK: "An NMR retrospective."
18:30 - 20:00 Poster session I - Even Better than the Real Thing. Presenters of EVEN numbered posters should be available at their poster during this time. (Drinks and snacks available)
20:00 - 22:00 Dinner
Tuesday, September 19th
09:00 - 10:35 Let’s Dance - Reaction monitoring and kinetics
Chair: Guy Lloyd Jones, The University of Edinburgh
"The session will cover the study of the mechanisms of organic and inorganic reactions and processes using in situ NMR techniques. The reacting systems investigated will demand the use of high and medium field NMR spectrometers for the analysis of reaction kinetics, the identification of reactive intermediates, and the quantitation of physical and thermodynamic reaction parameters. Also covered will be the development of new devices and tools for in situ reaction monitoring, both in flow and in static regimes, and methodologies for the efficient processing and analysis of the resultant high-density data. The session, which will cover the state of the art in a burgeoning field, will be of great interest to industry and academia."
Ulrich Hintermair, University of Bath, UK: Catch Me If You Can - Watching Homogeneous Catalysis with Real-time High Resolution FlowNMR
Erik von Harbou, University of Kaiserslautern, Germany: Quantitative NMR Spectroscopic Study of Highly Diluted Key Components in Complex Reactive Mixtures: Aqueous Amine Solutions Loaded with CO2
Jonas Kind, Technische Universität Darmstadt, Germany: Chances and Pitfalls of In-Situ Irradiation NMR Spectroscopy
Ludmilla Guduff, ICSN-CNRS, Gir-sur-Yvette, France: Ultrafast DOSY NMR of Hyperpolarised Mixtures (upgraded poster)
10:35 - 11:00 Break
11:00 - 12:35 We will rock you - Solid-state NMR applications
Chair: Steven Brown, The University of Warwick
"The last ten to twenty years have seen rapid advances in solid-state NMR research, in both hardware, especially ever faster magic-angle spinning (MAS), and pulse sequence development. Notably, while 13C cross-polarisation (CP) MAS is still a workhorse experiment, high-resolution two-dimensional homo- and heteronuclear 1H solid-state NMR spectra can be routinely obtained. Different pulse sequences utilise J and dipolar couplings to probe through-bond connectivities and through-space proximities. In the NMR crystallography approach, solid-state NMR experiment is combined with calculation of NMR parameters, usually with the density-functional theory (DFT) based GIPAW method for periodic solids. Applications to small molecules include organometallics, pharmaceuticals and supramolecular chemistry."
Ann-Christin Poeppler, Universität Würzburg, Germany: No Heavy Metal - NMR Crystallography of Metal Salts and Organometallic Compounds
Pierre Thureau, Marseille, France: Investigation of Powders at Natural Isotopic Abundance using Solid-State NMR and Dynamic Nuclear Polarization
Luis Mafra, University of Aveiro, Portugal: Combined Solid-State NMR, Diffraction and Modeling Studies of Small Molecule Pharmaceuticals
Kanika Sarpal, College of Pharmacy, University of Kentucky, Lexington, Kentucky, USA: Insights into Amorphous Solid Dispersion of Felodipine Using Solid-state NMR Spectroscopy: Miscibility and Molecular Interactions (upgraded poster)
12:35 - 18:00 Lunch followed by free afternoon
17:00 - 18:00 Round table discussion on NMR data reporting (not a formal SMASH program event)
This will be a roundtable discussion (Damien Jeannarat, Chair) based around a number of ongoing initiatives in creating and NMR data storage/reporting standards. These include Damien's NMRedata initiative (www.nmredata.org) and there are also RSC and IUPAC discussion around this topic. All SMASH attendees are welcome.
18:00 - 19:30 Poster session 2 - Against All Odds. Presenters of ODD numbered posters should be available at their poster during this time. (Open bar and light buffet menu of starters)
Wednesday, September 20th
09:00 - 10:35 Should I stay or should I go?- Non-covalent interactions and complexes
Chair: Elisabetta Chiarparin, AstraZeneca
"Small-molecule drug discovery is focused on occupancy of a protein binding site that directly affects protein function. This session will focus on versatile ligand based NMR methods to derive structures of free and bound ligands as well as their binding affinity and kinetics to aid lead generation and structure based drug optimisation."
Ben Davis, Vernalis, UK: Fragment Evolution Without Routine Crystallography
Julien Orts, ETH, Switzerland: NMR2 for Fast 3D Structure Determination of Protein-Ligand Binding Site Without Protein Resonance Assignment
Rodrigo Carbajo, AstraZeneca, UK: NMR Free Ligand Conformations for Enhanced Structure Based Drug Design
Serena Monaco, School of Pharmacy, University of East Anglila, Norwich, UK: DiffErential EPitope Mapping- (DEEP)STD NMR to Reveal the Pharmacophore of a Protein Target (upgraded poster)
10:35 - 11:00 Break
11:00 - 12:35 It’s not unusual - Multinuclear and inorganic methods
Chair: Michael John, Georg-August Universität Göttingen
"This session will focus on applications of NMR to small molecules outside the usual scope of H/C/N/F/P methods. It will cover both solution and solid-state NMR experimental results as well as quantum chemical calculations of NMR parameters. The objects of investigation are organometallic and inorganic systems, potentially including paramagnetic metals or quadrupolar nuclei. The session is intended to make this exciting and expanding field of research more familiar to the NMR community."
Markus Enders, University of Heidelberg, Germany: NMR Analysis of Small Paramagnetic Metal Complexes with Large Hyperfine Shifts
Pierre Florian, CEMHTI-CNRS Orleans, France: Elucidation of the Topological and Chemical Order in Materials by Multi-Nuclear Solid-State NMR
Armando Navarro-Vázquez, Universidade Federal de Pernambuco, Recife, Brazil: A Hyphenated Computational Protocol for Analysis of Natural Abundance 2H Residual Quadrupolar Couplings in (Chiral) Oriented Solvents
Olga Semenova, Center of Hyperpolarisation of Magnetic Resonance, Chemistry Department, University of York, York, UK: Hyperpolarised Low-Field NMR for Industrial Reaction Monitoring (upgraded poster)
12:35 - 14:00 Lunch
14:00 - 15:00 Workshop 3: We can work it out- Calculation of structures and NMR parameters
Chair: Giuseppe Bifulco, Università di Salerno
"The recent progress in the fields of NMR and of quantum chemistry has contributed to a great acceleration in the structural determination of complex organic molecules. Recently, the substantial potential offered even from the common personal computer has made possible the use of DFT methods in the optimization of the geometries and calculation of the properties of medium and high molecular weight compounds. For this reason the world of quantum chemical NMR parameter calculation has attracted the interest not only of the theoretical chemists, but also of the experimental NMR spectroscopists. In this workshop the structural study of organic compounds by means of an integrated DFT-NMR approach will be described. In particular, both theoretical and practical aspects of NMR parameter calculation by quantum mechanical methods will be discussed, with special regard toward the modern protocols involved in the structural and stereochemical assignment of natural and synthetic organic compounds. Questions regarding problems/limitations/future directions are encouraged during the workshop."
15:00 - 15:30 Break
15:30 - 17:05 Go your own way - Past SMASH hot topics revisited
Chair: Christina Thiele, Technische Universität Darmstadt
"Surprise, surprise ! This session will cover topics that were discussed in detail in previous SMASH meetings, but which did not make it onto the programme now for some time. Topics such as wide-band pulses and techniques for small scale samples are examples of what will be covered in this wide ranging session. We encourage those of you whose research might be in scope of this session to submit an abstract for a talk or poster!"
Burkhard Luy, Karlsruhe Insitut für Technologie, Germany: Broadband Pulses Revisited
Aldrik Velders, Wageningen University, Netherlands: Small Microcoils Are Still Hot
Sarah Robinson, Genentech, South San Francisco, USA: Hot Blooded, Check Out CPMG
Davy Sinnaeve, Department of Organic and Macromolecular Chemistry, Ghent University, Ghent, Belgium: General Approach to Access Long-Range 1H-1H RDCs (upgraded poster)
17:05 - 17:15 Closing Remarks
Thursday, September 21st (NB This is not a formal SMASH event)
09:30 - 15:30 qNMR Minisymposium - Registration (external link)!
Chair: Michael Maiwald (BAM) and Michael Bernstein (Mestrelab)
"Quantitative NMR (qNMR) is enjoying strong interest and rapid uptake. In recent times we have seen all the “pieces” for this analysis become easier to perform, covering a wide range of analytical requirements. Statistical error analysis and careful metrological studies make the method a serious contender to classical, chromatographic methods – even in highly regulated environments. Advances in NMR experiment design through to software analysis all add to the method’s robustness."
The principle themes of the Minisymposium will be:
- How: the practicalities of implementation
- When: applicability and validation
- Enabling: what’s available to help implementation
- Off-the-shelf: brief descriptions or demonstrations of manufacturers’ related products
- A more detailed outline agenda will become available soon
Note: Thanks to generous sponsorship, there is no cost to attend the meeting. Lunch and coffee break included!