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What's new at the NMR Facility

2010-2011 Annual Report (Jan 24/12) the 2010/11 Annual Report of the 900 NMR Facility has been finalized and is now available for download. We would like to thank all who contributed to this report, and to acknowledge our many users, clients, partners and funding agencies for continuing support of the 900 project.

124) Robert J. Attrell, Cory M. Widdifield, Ilia Korobkov, and David L. Bryce, "Weak Halogen Bonding in Solid Haloanilinium Halides Probed Directly via Chlorine-35, Bromine-81, and Iodine-127 NMR Spectroscopy," Crystal Growth and Design 12 (2012) accepted. http://dx.doi.org/10.1021/cg201683p

123) Luke A. O'Dell, Christopher I. Ratcliffe, Xianqi Kong, and Gang Wu, "Multinuclear Solid-State NMR and DFT Characterization of Interaction Tensors in Taurine," J. Phys. Chem. A 116 (2012) accepted. http://dx.doi.org/10.1021/jp210844t

122) C.M. Widdifield, T. Jurca, D.S. Richeson, and D.L. Bryce, "Using 69/71Ga Solid-State NMR and 127I NQR as Probes to Elucidate the Composition of "GaI"," Polyhedron (2012) accepted.

121) Kevin M.N. Burgess, Ilia Korobkov, and David L. Bryce, "A Combined Solid-State NMR and X-ray Crystallography Study of the Bromide Anion Environments in Triphenylphosphonium Bromides," Chemistry - A European Journal 18 (2012) accepted.

For other publications enabled by the 900 NMR Facility see complete list

The National Ultrahigh-Field NMR Facility for Solids and Bruker Canada are pleased to present the 7th Annual Solid-State NMR Workshop at the 95th Canadian Chemistry Conference and Exhibition in Calgary (CSC 2012). The workshop will take place on Saturday, May 26, 2012, 13:00 - 19:00.

This annual Canadian solid-state NMR event focuses on the latest developments in solid-state NMR spectroscopy with emphasis on practical aspects and applications in materials and life sciences. The workshop will be of interest not only to NMR spectroscopists, but also to students and other researchers interested in using modern NMR techniques in their research practice.

The current low nominal user fees have been in place since 2005 thanks to a generous CFI Infrastructure Operating grant. Due to the conclusion of this non-renewable grant there will be an increase in the user fees effective October 1, 2011 as follows:

The Steering Committee would like to point out that the increased Canadian academic rate still only covers a fraction of the operating costs of the facility.

The student travel grant program has temporarily been suspended until new funding sources are identified.

If you have any questions or concerns, please contact any member of the Facility Steering Committee.

Canadian Journal of Chemistry, Volume 89, Number 7 (2011) (part 1 of 2) http://www.nrcresearchpress.com/toc/cjc/89/7 Canadian Journal of Chemistry, Volume 89, Number 9 (2011) (part 2 of 2) http://www.nrcresearchpress.com/toc/cjc/89/9 David Bryce, Gang Wu, Yining Huang, "Tribute: Professor Roderick E. Wasylishen," Canadian Journal of Chemistry 89 (2011) xi-xvi. (Special Issue) http://dx.doi.org/10.1139/v11-067

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Cover article in Physical Chemistry Chemical Physics (July 4/11)

Cory M. Widdifield, Alex D. Bain, and David L. Bryce, "Definitive Solid-State 185/187Re NMR Spectral Evidence for and Analysis of the Origin of High-Order Quadrupole-Induced Effects for I = 5/2," Physical Chemistry Chemical Physics 13 (2011) 12413-12420. (Cover Article) http://dx.doi.org/10.1039/c1cp20572b

This is the tenth cover article featuring results obtained using resources of the National Ultrahigh-Field NMR Facility for Solids. See our cover gallery and the complete list of research publications enabled by the Facility here (complete list).

the Facility International Advisory Board meeting took place on June 5, 2011 during CSC 2011 in Montreal.

From NMR of Liquids and Gases to Solids - reflections of an ardent fan

Roderick E. Wasylishen

Gunning-Lemieux Chemistry Centre, University of Alberta, Edmonton, Alberta, T6G 2G2

Nuclear magnetic resonance spectroscopy is arguably the most powerful and diverse research tool available to scientists. NMR may be used to investigate atoms or molecules in the gaseous, liquid or solid state and has many useful applications. For example, the NMR technique can be used to map water density in the human body (MRI) or in fuel cells, measure hemodynamic response related to neural activity in the human brain (functional MRI), probe the three-dimensional structure of biological macromolecules in solids and liquids, assist synthetic chemists during the preparation of complex organometallic catalysts, provide information about the structure of solid materials that are not amenable to X-ray diffraction, and characterize hydrocarbon reservoirs in situ (NMR well logging). I first became fascinated by NMR spectroscopy because of the tight link between spectroscopy and quantum theory; one could analyze complex high-resolution NMR spectra using relatively simple quantum mechanical procedures. In this presentation I will review some of the progress in the field of NMR and focus on recent efforts to investigate little-studied and considered difficult quadrupolar nuclei such as 69/71Ga, 75As, 87Sr, 113/115In, and 121/123Sb via solid-state NMR. While NMR studies of such isotopes remain challenging, the use of moderate to high magnetic field strengths together with various signal enhancement techniques makes these studies feasible and is leading to interesting applications in inorganic and organometallic chemistry. I will provide a brief tour of the NMR periodic table as it pertains to non-integer spin quadrupolar nuclei, focusing on the importance of using high magnetic field strengths.

Prof. Roderick Wasylishen is spending his sabbatical (February-June 2011) in Ottawa, at NRC's Steacie Institute for Molecular Sciences and the National Ultrahigh-Field NMR Facility for Solids. Photo (L-R): Luke O'Dell, Jamie Bennett, Andreas Brinkmann, Rod Wasylishen, Igor Moudrakovski, Victor Terskikh, Eric Ye.

The National Ultrahigh-Field NMR Facility for Solids and Bruker Canada are pleased to present the 6th Annual Solid-State NMR Workshop at the 94th Canadian Chemistry Conference and Exhibition in Montreal (CSC 2011). The workshop will take place on Sunday afternoon, June 5, 2011 in the Palais des congrès de Montréal.

This annual Canadian solid-state NMR event focuses on the latest developments in solid-state NMR spectroscopy with emphasis on practical aspects and applications in materials and life sciences. The workshop will be of interest not only to NMR spectroscopists, but also to students and other researchers interested in using modern NMR techniques in their research practice.

Download the Workshop Program and Abstracts (PDF)

Workshop program

Session 1 (Palais, room 513D)
Chair Andreas Brinkmann (NRC Canada)

13:00-13:25 Stephen Hartman (Brock University) "NMR Studies of Nitrogen- and Aluminum-doped Silicon Carbide Polytypes"

13:25-13:50 Luke O'Dell (Steacie Institute for Molecular Sciences, NRC Canada) "New Possibilities for 14N Overtone NMR Spectroscopy"

13:50-14:15 Yining Huang (University of Western Ontario) "67Zn Solid-State NMR Characterization of Zn Environments in Metal-Organic Frameworks"

14:15-14:40 Frank Engelke (Bruker Germany) "A Brief Discourse on Magic Angle Spinning Technology"

14:40-15:00 Coffee Break

Session 2 (Palais, room 513D)
Chair Gang Wu (Queen's)

15:00-15:25 Alexandre Arnold (Université du Québec à Montréal) "Structure Determination of Collagen and Silk-Type Environments in the Blue Mussel Mytilus Edulis Byssal Threads"

15:25-15:50 Patrick Walsh (The Hospital for Sick Children, University of Toronto) "Solid-State NMR Characterization of a Soluble Prion Protein Octamer"

15:50-16:15 Karen Johnston (University of Windsor) "A 35Cl Solid-State NMR Study of Transition-Metal Organometallic Complexes Using Ultra-High Field NMR"

16:15-16:40 Robert Attrell (University of Ottawa) "Chlorine-35 and Bromine-81 Solid-State NMR Spectroscopic Study of Haloanilinium Halide Salts"

16:45 Reception sponsored by Bruker Canada

The purpose of this applet is similar to the popular Bruker’s pulse program, however the initial parameter input is manual, i.e. does not automatically use p1 (us) and pl1 (dB) values from the currently open dataset. Please enquire if you would like to test this applet and to provide your comments and suggestions. Email: Victor.Terskikh@nrc-cnrc.gc.ca

Physical Chemisty Chemical Physics has announced that the Canadian Society for Chemistry (CSC) is now one of its co-owner societies. To celebrate this new partnership, PCCP has created a collection of 25 top cited articles from authors based in Canada to showcase some of the great Canadian research published in PCCP. Five articles on this list are from Canadian solid-state NMR research groups, including four papers enabled by the National Ultrahigh-Field NMR Facility for Solids.

C.M. Widdifield and D.L. Bryce, "Crystallographic Structure Refinement with Quadrupolar Nuclei: a Combined Solid-State NMR and GIPAW DFT Example Using MgBr2," Physical Chemistry Chemical Physics 11 (2009) 7120-7122. http://dx.doi.org/10.1039/b911448n

D.H. Brouwer, S. Alavi and J.A. Ripmeester, "NMR Crystallography of p-tert-Butylcalix[4]arene Host-Guest Complexes Using 1H Complexation-Induced Chemical Shifts," Physical Chemistry Chemical Physics 10 (2008) 3857-3860. (Cover Article) http://dx.doi.org/10.1039/b805326j

L.A. O'Dell and R.W. Schurko, "Static solid-state 14N NMR and computational studies of nitrogen EFG tensors in some crystalline amino acids," Physical Chemistry Chemical Physics 11 (2009) 7069-7077. http://dx.doi.org/10.1039/b906114b

S. Cadars, D.H. Brouwer and B.F. Chmelka, "Probing local structures of siliceous zeolite frameworks by solid-state NMR and first-principles calculations of 29Si–O–29Si scalar couplings," Physical Chemistry Chemical Physics 11 (2009) 1825-1837. http://dx.doi.org/10.1039/b815361b

M.A.M. Forgeron and R.E. Wasylishen, "Molybdenum magnetic shielding and quadrupolar tensors for a series of molybdate salts: a solid-state 95Mo NMR study," Physical Chemistry Chemical Physics 10 (2008) 574-581. http://dx.doi.org/10.1039/b713276j

2009-2010 Annual Report (Nov 27/10) the 2009/10 Annual Report of the 900 NMR Facility has been finalized and is now available for download. We will start mailing printed copies shortly. We would like to take this opportunity to thank all our users and clients, as well as our partners and funding agencies for continuing support.

Congratulations go to a long-time 900 Facility user Vladimir Michaelis who has just defended his Ph.D. Thesis! Well done, Vlad!

Vladimir Michaelis (Department of Chemistry, University of Manitoba) November 10, 2010
Supervisor: Prof. Scott Kroeker
Ph.D. thesis "Nuclear Magnetic Resonance Studies of Disorder and Local Structure in Borate and Germanate Materials"

Vlad and Scott just published an important paper on 73Ge solid-state NMR in the Journal of Physical Chemistry which was part of his thesis project

90) Vladimir K. Michaelis and Scott Kroeker, "73Ge Solid-State NMR of Germanium Oxide Materials: Experimental and Theoretical Studies," Journal of Physical Chemistry C (2010) ASAP. http://dx.doi.org/10.1021/jp1071082

Speaker: Prof. Igor Mastikhin, University of New Brunswick, Fredericton

Title: "MRI of cavitation and other strange things"

Date: Thursday, November 18th, 2010

Time: 1:30 pm

Location: M-40, Montreal Road

Low concentration and poor sensitivity often hinder or make impossible solid-state 17O NMR in large biomolecular systems. In this cover article in Angewandte Chemie Gang Wu (Queen’s) and co-workers from the University of Ottawa and NRC Canada show that at an ultrahigh magnetic field of 21 T the high quality solid-state 17O NMR spectra can be obtained for large protein–ligand complexes of up to 300 kDa in size. Complementary multinuclear 17O, 27Al, and 13C NMR data obtained in this work have aided in the structural refinement for an ovotransferrin bound Al-oxalate complex.

Jianfeng Zhu, Eric Ye, Victor Terskikh, and Gang Wu, "Solid-State 17O NMR Spectroscopy of Large Protein-Ligand Complexes," Angewandte Chemie International Edition 49 (2010) 8399-8402. (Cover Article) http://dx.doi.org/10.1002/anie.201002041

Softpedia, November 18, 2010
Molecular Oxygen Studies Targeted by New Tool
(online)

Queen's University News Center, November 17, 2010
Scientists discover new method for studying molecules
(online)

This is an ninth cover article featuring results obtained using resources of the National Ultrahigh-Field NMR Facility for Solids. See our cover gallery and the complete list of research publications enabled by the Facility here (complete list).

David Bryce (University of Ottawa) has written a Perspective for Dalton Transactions about recent advancements in 43Ca NMR spectroscopy and its applications in materials science. David L. Bryce "Calcium Binding Environments Probed by 43Ca NMR Spectroscopy," Dalton Transactions 39 (2010) 8593-8602. (Cover Article). http://dx.doi.org/10.1039/c0dt00416b

This Perspective is featured on the cover of the current Dalton Transaction issue (2010, #37), and was recently highlighted by SpectroscopyNow

This is an eighth cover article featuring results obtained using resources of the National Ultrahigh-Field NMR Facility for Solids. See our cover gallery and the complete list of research publications enabled by the Facility here (complete list).

Dear NMR Facility Users:

we are preparing our 2009-2010 Annual Report and we would like to receive the following information from you by the August 15th deadline:

1) a brief progress report for each of your research projects. Please prepare a separate report for each project, regardless of whether the project has ended or not. Each report should illustrate for non-NMR specialists major project findings and should normally not exceed one-two pages (text and figures) (preferably MS Word format, or an ASCII text + figures separately). Selected progress reports will be included in the printed version of the Annual Report (previous reports)

2) all 2009-2010 research publications featuring results from the 900 instrument (published, accepted, submitted)

3) invited lectures and oral presentations in 2009-2010

4) poster presentations in 2009-2010

5) 2009-2010 : Honor thesis, Ph.D. thesis and similar works by your students using the 900 results (please indicate name of the student, department, title of thesis, date of the defense)

6) any other relevant information you may consider useful including in our report

Let me know if any questions, and thank you for your contribution!

On behalf of the Facility Steering Committee,

Victor Terskikh (E-mail)

Calcium is an important component in diverse materials and biochemicals. However, NMR spectroscopy of the only spin-active calcium isotope, Ca-43, is notoriously challenging due to its low natural abundance (0.14 %), low resonance frequency, and quadrupolar nature. Recently, researchers from the University of Ottawa, the NRC Steacie Institute for Molecular Sciences (SIMS-NRC), and Dalhousie University have independently reported advances in studies of inorganic polymorphs and cement-based materials using Ca-43 solid-state NMR spectroscopy.

"In spite of the great complexity of the calcium silicate chemistry involved in the hydration of Portland cement, we have shown that Ca-43 solid-state NMR provides useful new insights into cement chemistry", says Igor Moudrakovski (SIMS-NRC) of his collaboration with the Institute for Research in Construction (SIMS-IRC). Josef Zwanziger (Dalhousie) and his academic and industrial partners have similarly applied Ca-43 NMR in their project on the development, optimization and commercialization of high performance cement based composite materials.

Zwanziger explains, "we are trying to understand the nature of the composite-cement interface, and the mechanisms of toughening and strengthening in concrete composites. Calcium NMR is one of the many tools which is shedding light on the nature of the interface." At the University of Ottawa, David Bryce and his research group have demonstrated the utility of calcium NMR in understanding polymorphism in solids. This work has implications for understanding biomaterials as well as inorganic materials.

Because Ca-43 NMR in solid state requires a very strong magnetic field for sensitivity reasons, all these experiments were carried out at the National Ultrahigh-Field NMR Facility for Solids, a national user facility managed by the University of Ottawa and housed on NRC's Ottawa campus, which houses Canada's only 21.1 T (900 MHz) NMR spectrometer.

The latest calcium NMR research has been published in PCCP and J. Am. Chem. Soc., and a perspective on the state of the field is now available in Dalton Transactions (Bryce, 2010).

David L. Bryce "Calcium Binding Environments Probed by 43Ca NMR Spectroscopy," Dalton Transactions (2010) online. http://dx.doi.org/10.1039/c0dt00416b

Igor Moudrakovski, Rouhollah Alizadeh, James J. Beaudoin, "Natural abundance high field 43Ca solid state NMR in cement science," Physical Chemistry Chemical Physics 12 (2010) 6961-6969. http://dx.doi.org/10.1039/c000353k

David L. Bryce, Elijah B. Bultz, and Dominic Aebi, "Calcium-43 Chemical Shift Tensors as Probes of Calcium Binding Environments. Insight into the Structure of the Vaterite CaCO3 Polymorph by 43Ca Solid-State NMR Spectroscopy," Journal of the American Chemical Society 130 (2008) 9282–9292. http://dx.doi.org/10.1021/ja8017253

The National Ultrahigh-Field NMR Facility for Solids wishes to extend its sincere thanks to Yining Huang (Western), the outgoing member of the Facility Steering Committee who served in 2006-2010. Yining has done a great job as the representative for Ontario Universities. His valuable insights and suggestions have certainly helped to improve the Facility and broaden its userbase.

The Facility is pleased to announce that Gang Wu (Queen's) has been appointed to serve on the Facility Steering Committee as the representative for Ontario Universities for the next three years. Gang Wu is a long-time facility user and his first-hand experience will be very useful in managing the Facility. Welcome aboard, Gang!

To contact members of the Facility Steering Committee

the Facility International Advisory Board meeting took place on May 30, 2010 during CSC 2010 in Toronto.