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Magnetic Resonance (NMR and EPR)

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Magnetic Resonance (NMR and EPR)

Welcome to the OU NMR Facility

The NMR Facility is located near the east entrance of Stephenson Life Sciences Research Center. We provide training and access to all researchers who wish to use our instrumentation. In addition to researchers within the Department of Chemistry and Biochemistry, we are open to research groups from outside our department and outside the University of Oklahoma.

NMR Facility       NMR Personnel       Instrumentation       Training Policies     

Helpful links        Virtual NMR       Publications

NMR Facility

Our facility houses three Varian NMR Spectrometers and a Bruker EPR.

Interior of processing room
Data acquisition and processing is done in a separate room
Students working at work-stations in lab
A small wet lab with a ventilation hood is available for sample preparation
Photo of a room within the NMR facility

NMR Facility Personnel

Photo of Dr. Susan Nimmo

Dr. Susan L. Nimmo
NMR Facility Manager
Stephenson Life Sciences Research Center, room 1703

Email: SusanA@ou.edu

Phone: (405) 627-7044 (cell)
            (405) 325-0677 (office)
            (405) 325-2843 (NMR Lab)

Mailing Address: 

University of Oklahoma
Department of Chemistry and Biochemistry
NMR Facility
101 Stephenson Parkway
Norman, Oklahoma 73019

Instrumentation

VNMRS 500 MHz-NMR Spectrometer

The 500 NMR spectrometer was originally purchased as a VXR model in 1987 and was completed upgraded to a VNMRS model by the University in 2006 with the addition of Dr. Susan Schroeder and Dr. Robert Cichewicz to the Department of Chemistry and Biochemistry Faculty.

Photo of VNMRS 500-MHz-NMR Spectrometer

The spectrometer is a three channel, 28 shims Varian VNMRS-500 equipped with two probes: triplet resonance H{13C/15N} PFG probe, and a tunable indirect detection 1H{15N-31P} PFG probe.


VNMRS 400 MHz NMR Spectrometer

The 400 MHz NMR was originally purchased as a Varian Unity/Inova model in 1994 and was completely upgraded to the Varian VNMRS model in October, 2007 under the NSF Multi-user Grant # 0639199.

Photo of VNMRS 400-MHz-NMR Spectrometer

The system is complete with robotic sample insertion, automatic tuning and variable temperature accessories.  FTS air dryer provides dry air with a dew point of -85oC to the FTS preconditioning sample Cooler.  There is an available nitrogen gas source for applications below -85oC. The system is equipped with two probes:  a auto-tunable indirect detection 1H{15N-31P} PFG probe and a auto-tunable Dual Broadband 15N-31P {1H} PFG probe optimized for broadband detection.  Both probes are compatible with the auto-tuning accessory.   The dual broadband probe is the standard probe left on the magnet at all times.  Arrangements can be made to change the probe to the indirect detection probe upon request.  


Mercury VX-300 NMR Spectrometer

The 300 MHz NMR was purchased in 2000 under a NSF multi-user grant.  It operates with a 4-nuclei autoswitchable PFG probe. It can collect 1H/19F/13C/P31 without retuning the probe.

Photo of Mercury VX-300 NMR Spectrometer

This instrument is designed for walk-up use and is primarily used by the synthetic chemistry groups.  Mornings, Evenings and Overnight time can be reserved in advance in large blocks, but daytime can only be reserved in 15 minute blocks.


Bruker EMX EPR Spectrometer

 

Photo of Bruker EMX EPR Spectrometer

Training Policies

All students will begin training on the 300 NMR.  Training sessions will be approximately 45 minutes in duration and will be held as many times as necessary for the student to gain competency.  More advanced students and post-docs may gain certification by demonstrating their ability to use the instruments and by completing the assignments.

Certification to use the 300 NMR will be given as NMR Test #300-1, Test #300-2 and Practical Assignments #300-1 and #300-2 are completed as approved by Dr. Nimmo.

Training will begin on the 400 upon successful completion of 300 training. Certification to use the 400 NMR will be given as NMR Test #400-1, and Practical Assignments #400-1 and #400-2 are completed as approved by Dr. Nimmo.

Training will begin on the 500 upon successful completion of 400 training and Test #500-1. Certification to use the 500 NMR between 8-5 Monday-Friday will be given as NMR Test #500-2 is completed as approved by Dr. Nimmo. Unlimited access will be given upon the completion of NMR Test #500-3

Additional training may be requested on an individual basis. The training here represents the most basic and common use of the spectrometers in our department.

Variable temperature training will be given as needed.  Supervision of variable temperature experiments will continue until both the NMR facility manager and the student are completely confident of the student's ability to safely carry out these experiments independently.

All students will be provided a NMR Facility User Manual which details policies and gives step by step instuctions for operation of the instruments.  A pdf of this manual can be downloaded from the following link: NMR Facility User Manual (pdf)
 

NMR Facility Helpful Links

Instrument time is scheduled using the Faces On-line NMR Time Sign-up web page.  Our group name is OU-NMR.  A username and password will be provided to each user at the initial training session.

University of Oklahoma NMR Facility User Manual (pdf)

The Basics of NMR by Joseph P. Hornak, Ph.D.
 

Virtual NMR at the University of Oklahoma


NSF CHE#0639199

Goal: Provide NMR access to regional undergraduate institutions

Several regional undergraduate institutions wish to improve the teaching of their students with NMR experiments; however they do not have access to instrumentation. We will provide resources to these undergraduate institutions much in the same way that the Pacific Northwest National Laboratory (PNNL) operates a virtual NMR facility. This program has been successful with regards to bringing high field NMR expertise to other institutions.

Regional undergraduate institutions have different needs than large research institutions. Undergraduate universities require virtual NMR facilities which are available to them with regards to training, proximity and instrument time. Our program will model PNNL in providing teaching and research opportunities to regional undergraduate institutions with the 400 MHz NMR, which is sufficient for our external user base.  We will provide additional benefit through on-site training, tours and demonstrations in addition to remote operation and observation of the NMR experiment. Samples will be mailed to the NMR laboratory where a graduate student assistant will make the NMR samples, load the samples into the autosampler and clean the tubes at the conclusion.

Success of the remote access by the Undergraduate institutions is heavily dependent on the availability and quality of training.  It is imperative that both the professors and the students understand how to properly use the instrument.  Therefore, four workshops will be hed for the purpose of training and collaboration of the professors.  the workshop will be divided into parts:  effective teaching technique discussions and NMR training.  The discussions will be led by an OU Organic Chemistry Faculty member, Dr. Mark Morvant and the instrument training will be conducted by the NMR facility manager, Dr. Susan Nimmo.  Training will continue throughout the year via remote screen sharing.

Photo of a workshop gathering in NMR Lab

The first workshop was held Tueday May 20, 2008 and was attended by faculty from Oklahoma Baptist University (Shawnee, Oklahoma), Oklahoma Christian University (Edmond, Oklahoma), Oklahoma City University (OKC, Oklahoma), East Central University (Ada, Oklahoma), Southern Nazarene University (Bethany, Oklahoma), and Southwestern Oklahoma State University (Weatherford, Oklahoma).

Publications

Sena Filho, J.G.; Nimmo, S.L.; Xavier, H.S.; Barbosa-Filho, J.M.; Cichewicz, R.H.; “Phenylethanoid and Lignan Glycosides from Polar Extracts of Lantana: A Genus of Verbenaceous Plants Widely Used in Tradititional Herbal Therapies”. Journal of Natural Products, 72(7), 2009, 1344-1347.

Guan R.; Nimmo S.L.; Schnackerz, K.D.; Cook, P.F.; “P-31 NMR studies of O-acetylserine sulfhydrylase-B from Salmonella typimurium”. Archives of Biochemistry and Biophysics, 487(2), 2009, 85-90.

Cook, P.; Lin, Y.; Volkman, J.; Nicholas, K,; Yamamoto, T.; Eguchi, T,; Nimmo, S.; West, A., "Chemical Mechanism of Homoisocitrate Dehydrogenase from Saccharomyces cerevisiae" Biochemistry,  2008, 47, 4169-4180.

Harwood, T.D.; Nimmo, S.L.; Kettle, A.J.; Winterbourn, C.C.; Ashby, M.T.; "Molecular Structure and Dynamic Properties of a Sulfonamide Derivative of Glutathione that Is Produced Under Conditions of Oxidative Stress by Hypochlorous Acid", Chemical Research in Toxicology 21(5), 1011-1016, 2008

Nimmo, S.L.A..; Lemma, K.; Ashby, M.T.; "Reactions of Cysteine Sulfenyl Thiocyanate with Thiols to Give Unsymmetrical Disulfides", Heteroatom Chem, 2007, 18, 467-471.

Lin, Ying; Alguindigue, S.S.; Volkman, J.; Nicholas, K.M.; West, A.H.; Cook, P.F.; "The Complete Kinetic Mechanism of Homoisocitrate Dehydrogenanse from Saccharomyces ceresvisiae", Biochemistry, 2007, 46, 890-898.

Xu, Hengyu, Alguindigue, S.S.; West, A.H.; Cook, P.F.; "A proposed Proton Shuttle Mechanism for Saccharopine Dehydrogenanse from Saccharomyces ceresvisiae", Biochemistry, 2007, 46, 871-882.

Lin, Ying; Alguindigue, S.S.; Volkman, J.; Nicholas, K.M.; West, A.H.; Cook, P.F.; "The Complete Kinetic Mechanism of Homoisocitrate Dehydrogenanse from Saccharomyces ceresvisiae", Biochemistry, 2007, 46, 890-898.

Xu, Hengyu, Alguindigue, S.S.; West, A.H.; Cook, P.F.; "A proposed Proton Shuttle Mechanism for Saccharopine Dehydrogenanse from Saccharomyces ceresvisiae", Biochemistry, 2007, 46, 871-882.

Nagy, P.; Alguindigue, S.S.; Ashby, M.T.; "Lactoperoxidase-Catalyzed Oxidation of Thiocyanate by Hydrogen Peroxide:  A reinvestigation of Hypothiocyanite by Nuclear Magnetic Resonance and Optical Spectroscopy", Biochemistry, 2006,

Smith, G.L.N.; Alguindigue, S.S.; Khan, M.A.; Powell, D.R.; Taylor, R.W.; "1H and 13C NMR assignments and x-ray structures for three monocyclic benzoannelated dilactam polyethers", Mag. Res. Chem., 2006, 901-904.

Rabeth, W.M.; Alguindigue, S.S.: Cook, P.F.; "Mechanism of the Addition Half of the O-Acetylserine Sulfhydrylase-A Reaction", Biochemistry, 2005, 44(13), 5541.

Zahran, Z.N., Lee, J., Alguindigue, S.S., Khan, M.A., Richter-Addo, "Synthesis, Characterization, and Molecular Structure of Six-Coordinate Manganese Nitrosyl Porphyrins". Dalton Trans. 2004, 1, 44.

Jiang, X.-R., Wronga, M. Z., Alguindigue, S. S., Dryhurst, G. "Reactions of the Putative Neurotoxin Tryptamine-4,5-Dione with L-Cysteine and other Thiols. Chem. Res. Toxicol., 2004, 17(3), 357.

Solh, C.D., Lee, J., Alguindigue, S.S., Khan, M.A., Richter-Addo, G.B. "Synthesis and Solid-State Molecular Structures of Nitrosoalkane Complexes of iron Porphyrins containing Methanol, Pyridine, and 1-Methylimidazole ligands". J. Inorg. Biochem. 2004, 98 (7), 1238.

Ashby, Michael T.; Alguindigue, Susan S.; Schwane, Justin D.; Daniel, Tad A.  "Regular and Inverse Secondary Kinetic Enthalpy Effects (KHE) for the Rate of Inversion of Thioether and 1,1'-Biisoquinoline Complexes of Ruthenium and Osmium" Inorg. Chem., 2001, 40(26), 6643.

Das, P.K.; Alguindigue, S.S.; Ashby, M.T.; "A DFT Study of Zr-S Rotational Barriers of (h5-C5H5)2Zr(Cl)(SR).  The Origin of an Inverse Steric Effect" Can J. Chem., 2001, 79(5/6), 809.

Ashby, M.T.; Alguindigue, S.S.; Khan, M.A.;  "Kinetic Element Effect for Atropisomerization of an Organometallic Complex of the Misdirected Ligand   1,1'-Biisoquinoline" Organometallics, 2000, 19, 547.

Alguindigue, S.S.; Khan, M.A.; Ashby, M.T.; "Syntheses and Molecular Structures of Ruthenium (II) Complexes of the Atropisomeric Ligands 1,1'-Biphenyl-2,2'-diamine and 3,3'-Diamino-2,2'-bipyridine" Inorg. Chim. Acta, 2000, 310(2), 156.

Alguindigue, S.S.; Khan, M.A.; Ashby, M.T.; "Kinetics and Mechanism of the Stereochemical Isomerization of an Arene-Ruthenium Complex of the Atropisomeric Ligand 1,1'-Biphenyl-2, 2'-diamine" Organometallics, 1999, 18, 5112.

Ashby, M.T.; Alguindigue, S.S.; "Modulating the Energetics of Electron Transfer with a Dynamic Misdirected Ligand:  A Model for Non-planar Heme", J. Inorg. Biochem., 1999, 74, 70.

Alguindigue, S.S.; Khan, M.A.; Ashby, M.T.; "Kinetics and Mechanism of the Stereochemical Isomerization of an Arene-Ruthenium Complex of the Atropisomeric Ligand 1,1'-Biphenyl-2, 2'-diamine" Organometallics, 1999, 18, 5112.

Ashby, M.T.; Alguindigue, S.S.; Khan, M.A.;  "Misdirected p-Donor Ligands: (h5-C5H5)2Zr(Cl)(SR) with Sterically More Demanding R Groups have Lower Rotational Barriers"  Inorg. Chim Acta, 1998, 270, 227.