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X-Ray Crystallography

About

The X-ray Crystallography facility offers a complete service for structure solution, refinement and powder diffraction analysis of small molecules, as well as a variety of software for structural analysis and graphics, including the Cambridge Structural Database and CrystalMaker. Low temperature data collection is possible for both single crystal and powder diffraction experiments.

Available equipment:

  • Two single crystal X-ray diffractometers (one Bruker APEX DUO equipped with Mo and Cu sources, and one Bruker X8 APEX equipped with a Mo source)

  • Two powder X-ray diffractometers (Bruker D8 Advance and Bruker D8 Discover equipped with a GADDS detector).

  • 7 PC workstations available for structure determination and refinement, and powder diffraction analysis.

Research fields we have assisted:

  • Chemistry
  • Environmental Science
  • Forensic Science
  • Fuel Cell Research
  • Materials Engineering
  • Mineralogy, Mining, and Earth Science
  • Pharmaceutical Science
  • Polymer Science
  • Wood Science

Contact:

For X-ray Crystallographic Services: Please contact Dr. Brian Patrick at the Structural Chemistry Facility at UBC for current charges for X-ray crystal structure determination.

Brian Patrick, Ph.D
Tel: (604) 822-4865
Fax: (604) 822-2847
Email: 

Our Members:

Dr. Brian Patrick,  , Manager
Anita Lam, 

 

Instruments

Bruker Apex DUO

  • Two X-ray sources: Mo and Cu 
  • Greater Mo intensity with the Triumph monochromator - useful for challenging or weakly diffracting crystals
  • High intensity Cu microsource radiation for the determination of absolute structures for light atom organic compounds
  • Automatic data collection strategy determined using COSMO, cell determination and integration carried out with SAINT (or CELL_NOW for twinned crystals)
  • Kappa geometry, allows for crystal orientation

 

DUO

Bruker X8 Apex CCD

  • Sealed tube Mo radiation with low temperature capability
  • Automatic data collection strategy determined using COSMO, cell determination and integration carried out with SAINT (or CELL_NOW for twinned crystals)
  • Kappa geometry, allows for crystal orientation

 

D8-Advance

  • For routine identification of powder and materials
  • Cu source with LynxEye detector
  • 9-position sample changer for automatic data collection
  • TOPAS software for advanced applications
  • Training available for both instrumental and software applications (please inquire)
D8 Advance

General Area Detector Diffraction System (GADDS)

(subject to availability)

  • Measure single particles or minute samples
  • Laser and video alignment pinpoints the analytical area of the sample
  • Capillaries available to measure colloidal suspensions, air-sensitive samples, or small amounts of powder
  • Non-destructive for precious samples
  • Ideal for looking at diffraction in 2-dimensional space such as for polymers and textured materials

 

  • GADDS GADDS
GADDS

Variable Temperature

(Please inquire)

  • Two different set-ups available
  • Customizable to suit different needs

Services

Services:

Database Access

X-Ray diffractometer sign up

Sample submission - Powder XRD:

Powder X-Ray Diffraction Sample Submissions

 

Sample submission - Single Crystal XRD:

Click here to print a Submission Form (Adobe PDF format).

Click here to view a sample of a completed submission form (Adobe PDF format).

 

How to keep the Crystallographer happy; some general rules and advice:

 

  1. Avoid submitting a polycrystalline mass of solid material. The sample should consist of carefully grown single crystals. A crystal is defined by straight edges and plane faces (see any crystallography text for further information). If your sample does not have the prerequisite morphology, the crystallographer would be happy to look at it, but keep in mind that you may have to recrystallize it.
    Crystals used in the diffraction experiment are typically no larger than 0.5 x 0.5 x 0.5 mm in each direction. X-ray quality crystals that are larger in dimension are cut by the crystallographer to a suitable size. Very small crystals can also be submitted to the crystallographer, but these samples may be too weakly scattering. In such cases, recrystallization to obtain larger crystals may be necessary if the diffraction experiment fails.
  2. Avoid submitting impure material. X-ray quality crystals should be grown purposely, and should not usually be derived from purification or characterization attempts (e.g. crystals coming from NMR tubes is discouraged).
  3. If crystals do not grow from one solvent, try another. Be aware that growing crystals from certain solvents may result in crystals containing disordered solvent, and this may impede the structure determination.
  4. Please ensure that the sample is sufficiently characterized by other methods so that its chemical formula is mostly correct. One of the most common mistakes is the submission of a material that is not what the chemist thinks it is .
  5. Devise a numbering scheme for the proposed molecule prior to sample submission, and include this numbering scheme with the submission form.
  6. Submitting air stable crystals in small sample vials is preferred, but not necessary. Samples submitted in round-bottomed flasks or other glassware that impedes optical examination and microscopic manipulation of the crystals are not preferred.Ê Air-sensitive materials can be submitted in any type of container.
  7. Evaporation of samples to dryness during recrystallization may result in the crystals adhering to the walls of the container. This may increase the likelihood that the crystals are crushed when the crystallographer attempts to isolate potential specimens.

Remember the old crystallographic saying: Garbage In = Garbage Out