Crystallography
Crystallography Facility Overview
The Virginia Tech Crystallography Lab (VTX) was formed by combining the resources of the Departments of Chemistry, Geosciences and Biology with support from the College of Science. VTX operates five diffractometers and is able to collect data on a broad range of single-crystal samples (e.g. small molecules, frameworks, minerals and proteins). The Department of Chemistry operates two diffractometers as part of a service center: the Rigaku Oxford Diffraction “Synergy” (NSF MRI Grant 1726077) and the Rigaku Oxford Diffraction “Gemini”.
| Instruments | Internal | Federal | External |
|---|---|---|---|
| Instrument Time | $9.90 | $15.90 | $125.00 |
| Tech Assist | $40.00 | $64.40 | $125.00 |
- Crystal screening and mounting
- Structure solution, refinemenet, and interpretation of chemical/minerals samples
- Cambridge Crystallographic Database searching
- Specialized Experiments (see below)
The diffractometers are designed for single-crystal samples. Other techniques (including powder diffraction) are considered ‘specialized’ and are only offered by special request and with adequate justification for the need of the single crystal instruments as opposed to instruments specifically designed for such experiments.
This must be done in collaboration with a protein crystallographer: VTX staff will gladly assist with data collection but we are not trained in protein crystallography. Users must be prepared to assist the crystallographer in the lab; structure solution and refinement services are NOT available.
VTX has the unusual capability to collect in-situ high-pressure single crystal data (up to 10 GPa). These experiments are highly specialized and are offered through research collaboration with Professor Nancy Ross.
The goal of the course is to provide students with a hands-on introduction to crystallography. The target audience is students who use crystallography as a tool in their research and who submit samples to the X-ray Service Center for analysis (but do not use crystallography enough to take the 2-semester course qualifying them to work independently).
Covers the means of describing a crystalline solid, including lattices and symmetry (i.e. 2D and 3D point groups, 2D plane groups, and 3D space groups), allowing for the formal description of structures and surfaces and the interpretation of published crystallographic data. This course is a prerequisite for CHEM 5526/GEOS 5536. Undergraduates who have taken CHEM 3615, GEOS 3504, or an equivalently rigorous course are welcome to register.
Covers diffraction theory and practical aspects of single-crystal and powder X-ray diffraction.
CHEM 5525/GEOS 5535 is a prerequisite. Students who complete this course are permitted to work independently in VTX.
Key Policies and Safety
Critical Safety Rules
DANGER: Projectile Hazard
- Never bring heavy ferromagnetic objects beyond the 5 Gauss line (marked around each magnet)
- Even small items (paper clips, bobby pins) will be attracted and can stick to the magnet impacting shims
- Heavy items (wrenches, scissors, chairs, gas cylinders) become dangerous projectiles
- Gas cylinders are absolutely prohibited unless staff authorized.
Medical Devices & Implants
STOP: If you have any of the following, you MUST get staff clearance before entering:
- Cardiac pacemakers or ICDs
- Cochlear implants
- Neurostimulators (deep brain, spinal cord, vagus nerve)
- Aneurysm clips
- Metallic foreign bodies (shrapnel, metal fragments)
"MRI Safe" ≠ "NMR Safe" — Our magnets operate at much higher fields (9.4-14.1 Tesla) than clinical MRI (1.5-3.0 Tesla)
- Remove mechanical watches before approaching magnet during sample insertion:
- Mechanical watches will be permanently magnetized and ruined
- Piercings and jewelry are generally safe, but take care if large and ferromagnetic
- NMR tube transport: Always use secondary containment (no glass containers)
- Magnet quench: If you hear loud roar/boom or see dense fog, leave immediately and contact NMR staff
- No drop-ins for staff assistance (email or call ahead)
- Instrument consoles: For acquisition only — process data offline on your computer
- Report all incidents: Spills, breakage, instrument issues, or safety concerns immediately
- Automated walkup operation: IconNMR (Bruker) or Delta interface (JEOL)
- Never work alone if handling potentially hazardous samples
- Know the location of emergency exits and safety equipment
- Keep your phone accessible for emergency communication
- If a magnet quench or safety incident occurs, evacuate immediately and contact NMR staff
Do NOT use chipped, cracked, or damaged NMR tubes.
Damaged tubes can:
- Cause instrument downtime and costly probe damage
- Get stuck in the magnet or autosampler
- Produce poor quality spectra
How to fill out an Analytical Services ISR
Supplier: "VT Chemistry X-Ray Lab"
Contact Ken Sharp-Knott
kknott@vt.edu
540-231-0885
When co-authorship is expected:
- Substantial intellectual contributions to experimental design, data interpretation, or manuscript preparation
- Specialized technique development or troubleshooting beyond routine support
- Custom method development, extensive troubleshooting, or data analysis assistance
When acknowledgment (not co-authorship) is sufficient:
- Routine training and instrument access
- Standard walkup experiments without significant staff involvement
- Minor troubleshooting or parameter adjustments
Best practice: Discuss authorship expectations early in your project with facility staff to avoid misunderstandings.
When describing your NMR experiments in the Methods or Experimental section of manuscripts, cite relevant instrument details from the Instruments page. Include:
- Instrument name (e.g., "Bruker Avance IV Neo 600 MHz")
- Probe type (e.g., "Prodigy TCI cryoprobe")
- Field strength and observe frequency
Example Citation:
"¹H and ¹³C NMR spectra were acquired on a Bruker Avance IV Neo 600 MHz spectrometer equipped with a Prodigy TCI cryoprobe. NMR data reported in this work were obtained at the Virginia Tech Chemistry NMR Facility (RRID:SCR_027587)."
- Specify solvent, temperature (if non-ambient), and spectrometer frequency
- Include coupling constants (J) in Hz for multiplets
- For quantitative NMR, describe relaxation delays, pulse angles, and any relaxation agents used
All data automatically uploaded to LOGS server:
URL: https://nmrsc.chem.vt.edu/asds
Login: Same credentials as FACES and instrument login
- Download datasets from LOGS to your local computer
- Process in MNova (facility standard software)
- Save MNova file (each file should contain experiments for ONE compound)
- Site license provided by facility
- Request license key via email
- Distributed automatically after training completion
- Must connect to VT network (eduroam or VPN) for validation
Virginia Tech has a site license to the Cambridge Structural Database. For occasional users of the database, the WebCSD can be accessed from any computer with a Virginia Tech IP address. Users who need frequent and/or specialized searches, or who need access to a CSD software suite (CSD-System, CSD-Materials, or CSD-Discovery) should contact Dr. Slebodnick for download instructions.
Laboratory Hours
Staffed Hours: 9a - 5p, M-F
24/7 access for trained users
Contact NMR Staff
Ken Sharp-Knott
NMR Facility Manager
kknott@vt.edu
540-231-0885
540-267-6502 (Emergencies Only)
Murthy Shanaiah, Ph.D.
NMR Spectroscopist
nmrns@vt.edu
540-231-8256
Emergency Contact
VT Environmental Health & Safety
540-231-5364
www.ehs.vt.edu
Kenny Smith
Facilities Manager
kesmith7@vt.edu
Drew Murphy
Safety Coordinator
drewmurphy23@vt.edu
Lab Address
Hahn Hall South 002
Virginia Tech
900 W. Campus Blvd.
Blacksburg, VA 24061