he NMR facility is a service and research laboratory operated by and for the Department of Chemistry at Indiana University. The laboratory performs and assists in magnetic resonance spectroscopy activities that further the research goals of departmental faculty, post-doctoral fellows, students, and staff. The following report summarizes the service and research activities of the NMR Facility during 19992000.

Regrettably, in March 2000 our long time staff member and assistant scientist of the Department, Dr. Marty Pagel, left the University to pursue his career at Monsanto Company. At Monsanto, Marty oversees the NMR facility and supervises other technical services. Marty has been instrumental in the upgrade of our NMR facility to its current state and has written the Web based MAGnet REServations software. We thank Marty for many years of his service.

From March on, the NMR facility has been understaffed: Between March and August, Dr. Ulrike Werner-Zwanziger and Jeff Frey oversaw the facility operation. Starting in summer Angela Hansen helped out part time while being trained. In August, John Tomaszewski joined the NMR Facility staff as Assistant Manager. His arrival coincided with the beginning of the sick leave of Ulrike Werner-Zwanziger (due to the premature birth of Clara Zwanziger). Until the end of the year 2000, John, Jeff and Angela oversaw the operation of the NMR facility. In November, Frank Gao joined the Department of Chemistry and served in the NMR facility on a part-time as needed base.

The NMR Facility includes the following NMR spectrometers dedicated for liquid samples:

• Varian Unity^INOVA spectrometer operating at a 500 MHz ¹H Larmor frequency (I500)
• Varian Unity^INOVA spectrometer operating at a 400 MHz ¹H Larmor frequency (I400)
• Varian VXR-Unity spectrometer operating at a 400 MHz ¹H Larmor frequency (VXR400)
• Varian Gemini-2000 spectrometer operating at a 300 MHz ¹H Larmor frequency (Gem300)

In addition the NMR Facility operates a spectrometer dedicated for solid samples:

• Bruker Avance spectrometer operating at a 400 MHz ¹H Larmor frequency (NMRSS1)

In conjunction, four Sun workstations, two SGI workstation, and seven Windows-NT and Linux workstations provide processing, simulation, and administrative capabilities in the NMR Facility laboratory. A variety of probes are available for the observation of all possible nuclei and for conducting a wide variety of multinuclear experiments.

In addition the NMR facility staff oversees and maintains a Gemini 200 NMR spectrometer serving the undergraduate teaching laboratories.

Non-routine research collaborations are development of new NMR techniques or interpretation of spectra beyond daily interactions between Staff and Users. Research collaborations in 2000 include

• highly resolved two-dimensional experiments for analyses of polymer compositions (Chisholm group), of paramagnetic molecules (Christou group), and of metal complexes (Caulton group)
• experiments observing ¹¹B (Todd group), ⁵¹V (Christou group), ²H (Christou, Caulton groups), and ²⁹Si (Caulton group)
• pulse sequence development and creation of macros (Stone group, Johnston group).
• multinuclear solid state NMR experiments for polymer characterizations (Zwanziger group)
• alignment studies in the solid and liquid crystalline state of Nickel and Zinc porphyrines (Chisholm and Zaleski groups)
• solid state experiments on solid/gas reactants (Caulton group)
• pulse sequence development for studies on phosphite glasses, conducting polymers and glass ceramics (Zwanziger group)

• Coalter III, J. N., Bollinger, J. C., Huffman, J. C., Werner-Zwanziger, U., Caulton, K. G., Davidson, E R., Gérard, H., Clot, E., & Eisenstein, O. Coordinated carbenes from electron-rich olefins on RuHCl(PPri3)2, New J. Chem., 24, 9-26 (2000)
• Goodman JL, Pagel MD, Stone MJ, Relationships between protein structure and dynamics from a database of NMR-derived backbone order parameters, J. Mol. Biol,. 295, 963-978 (2000)
• C. Joo, U. Werner-Zwanziger, and J. W. Zwanziger, The ring structure of boron trioxide glass, J. Non-Cryst. Solids, 261, 282-286 (2000) and 271, 265-266 (2000)
• C. Joo, U. Werner-Zwanziger, and J. W. Zwanziger, Anisotropy-correlated spectroscopy of quadrupolar nuclei, Solid. State. Nucl. Mag Res. 16, 77-83 (2000)
• C.G. Joo, U. Werner-Zwanziger, and J. W. Zwanziger, The boroxol ring fraction in boron trioxide glass, Phys. Chem. Glasses, 41, 317-320 (2000)

• Chisholm, M.H., Crandall, J.K., McCollum, D.G., & Pagel, M. Concerning the Mechanism of Ring-Opening polymerization by Coordinate Catalysts: The 2D Homonuclear J-Resolved Spectrum of Poly(cyclohexene oxide). Submitted for publication.

• Joo, C., Werner-Zwanziger, U., & Zwanziger, J.W., The Ring Structure of Boron Trioxide Glass, Solid State NMR, submitted

• Joo, C., Werner-Zwanziger, U., & Zwanziger, J.W., The Ring Structure of Boron Trioxide Glass, Journal of Non-Crystalline Solids, submitted

• Joo, C., Werner-Zwanziger, U., & Zwanziger, J.W., The Ring Structure of Boron Trioxide Glass, Conference Proceeding for …. submitted

• Shoemaker JL, Westen EA, Pagel MD, Prange HD The mechanisms underlying the chloride shift: II. PO2-dependent binding of chloride to hemoglobin in whole blood. FASEB J, 14 A438-A438 (2000).
• Ring Opening Polymerization of Cyclic Ethers and Esters by Aluminum Catalyst Precursors, B. Antelmann, M. H. Chisholm, J. C. Huffman, S. S. Iyer, D. Navarro, M. Pagel, U. Werner-Zwanziger, and W. Simonsick, PINDU 2000, Bloomington, Indiana, 2/12/00
• Magnetic Alignment of Some Metalloporphyrazine Liquid Crystals, H. Chisholm, B. D. Pate, U. Werner-Zwanziger and J. M. Zaleski, PINDU 2000, Bloomington, Indiana, 2/12/00

• U. Werner-Zwanziger, Solid-State NMR Methodology and Applications to Complex Materials, Naval Research Laboratory, Washington, DC, 5/19/00

• Inorganic chemists dominate utilization of the Gem300 and I400. Organic chemists dominate utilization of the VXR400. Biochemists dominate utilization of the I500. DatastationsData stations were used by a variety of research interests. Utilization of the I400 by organic chemists or of the VXR400 by inorganic chemists has not shifted the major user groups from their traditional use.

• Utilization of the I500 and NMRSS1 is extremely high. The I500 is efficiently used by the biochemists for large blocks of time. NMRSS1 is specialized on long duration solid state NMR experiments.

• The monthly use of the VXR400 is fairly even throughout the year. Increased use in May probably results from the end of the semester and a shift towards research activities. The departure of Professor Chisholm's group in summer 2000 impacted the use of the I400 and Gem300 NMR spectrometer. Their utilization dropped in the second half of the year after an increase just prior to the shrinking of his laboratory.

In the summer the Staff offered a series of "NMR meetings" discussing the practical aspects and background of NMR spectroscopy.

The Staff consulted with ESPE, Germany concerning the NMR spectroscopy of polymers.

MAG RES, the web-based magnet reservation and scheduling system, was distributed to national and international NMR Facilities.

The MAGnet REServation scheduling system was implemented for I400 scheduling in Feb. 1998, and implemented for scheduling other spectrometers in June 1998. This system allows users to reserve spectrometer time via web browsers, and replaced the paper-based system. A demo version of the MAG RES system and a freeware version were also made available via the NMR Facility web site.

The computer security was improved by upgrading several services and disabling others.

The quad probe of the I400 NMR spectrometer had to be repaired when a detection coil surrendered to the permanent friction from the spinning of the samples.

The Web pages were updated with various help and "how to" items in the "User’s Guide".

The improvement of the login speed is a high priority.

Proposals for funds for a departmental 600 MHz NMR spectrometer to NIH and NSF will be written.

The electronic and paper forms of our User Guides will be updated.

MAG RES will be improved::

• add rejection of reservation requests or deletions for time in the past

• add rejection of reservation requests that are longer than the maximum allowed length

• add rejection of reservation requests made too far in the future

• add signup possibilities for the new solid state NMR instrument

• incorporation of the new usage rules

• Perl scripts for automatic billing for the solid state NMR instrument will be written

• add installation script

• add JavaScript to initiate immediate action for certain pull-down menus and buttons

Data for the Graph Gallery was derived from NMR Facility accounting records from January, 1^st to December, 31^st 2000. 7These records were automatically generated from the spectrometer & datastation login/logout processes.