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Department of Chemistry

Science A 229
University of Calgary
2500 University Dr NW
Calgary, AB T2N 1N4 Canada
T. 403.220.5341
F. 403.289.9488
info@chem.ucalgary.ca

X-Ray Crystallography Services

X-ray crystallography is a highly sophisticated technique for extracting structural information from both single crystal and polycrystalline samples. All branches of scientific research can benefit from this technique. In certain cases, X-ray data provides the only solution to understanding the behavior of the whole system. Our X-ray Facility houses several X-ray diffractometers capable of producing highly accurate and reliable structural data for both single-crystals and polycrystalline samples.


Instruments and Devices

Single-Crystal X-Ray Diffractometers

Two single crystal X-ray diffractometers are housed in our X-ray Facility:

  1. Nonius Kappa APEX2 CCD (Figure 1) with Mo sealed tube (2.0 kW), 4-circle Kappa-geometry goniometer, and APEX2 1k CCD X-ray detector. Nonius suite of “Collect” is used for data collection and reduction.

    Figure 1. Core of the Nonius Kappa APEX2 CCD system
                                                   Figure 1. Core of the Nonius Kappa APEX2 CCD system

  2. Bruker SMART APEX2 CCD (Figure 2) with Cu sealed tube (1.5 kW), 3-circle fixed Chi goniometer, and APEX2 1k CCD X-ray detector. Bruker APEX II suite is used for data collection and reduction.

    Figure 2. Core of the Bruker SMART APEX2 CCD system
                                                        Figure 2. Core of the Bruker SMART APEX2 CCD system

Polycrystalline X-Ray Diffractometer

A Bruker D8 Advance (ECO) (Figure 3) powder X-ray diffractometer with highly sensitive Lynxeye XE energy dispersive 1D X-ray detector and Twin-Twin optic system was recently purchased and installed in the fall of 2016. The sample stage is fixed at θ = 0°, which makes mounting of a liquid sample easy; the X-ray source and detector are coupled in θ-θ mode, with 2θ ranging from 0 to 150°. A parallel X-ray beam is available for samples with an irregular surface, and programming slits allow identical footprints of X-ray beams on the surface of the sample.

     Figure 3. Core of the Bruker D8 Advance (ECO) system
                                                              Figure 3. Core of the Bruker D8 Advance (ECO) system

Cryogenics System

Two different sets of cryostats are installed on our Nonius Kappa APEX2 CCD system and Bruker SMART APEX2 CCD system, respectively:

  1. Oxford Cryosystems 700 open flow nitrogen cryostat with temperature range from 80 to 400 K.
  2. Oxford Cryosystems 700+ open flow nitrogen cryostat with temperature range from 80 to 500 K.

Users are encouraged to set the temperature according to the requirements of their experiments. Lower temperatures should be adopted when feasible to minimize the TDS; however, when humidity is high, you may observe fast formation of ice on the surface of the crystal. Use of cryostats is very helpful if you want to follow phase transitions with small amounts of powder sample. If necessary, the temperature can be calibrated to high accuracy.

Microscope

Two stereomicroscopes, namely Leica MS5 (Figure 4) and WILD HEERBRUGG (Figure 5.), are using in our X-ray lab for sample evaluation. The quantitative polar light stage is available on Leica MS5, which is very helpful to identify crystals that are twinned, as well as amorphous solids.
     Figure 4. Leica MS5      Figure 5. WILD HEERBRUGG
                                 Figure 4. Leica MS5                                                                       Figure 5. WILD HEERBRUGG


Software

A wide variety of software used in X-ray crystallography and access to the Cambridge Crystallographic Database, which contains over 700,000 crystal structures, are available in the X-ray Crystallography laboratory.


Rates

We offer frames, data, and structures for single crystal X-ray diffraction; patterns and results based on whole pattern profile fitting and/or Rietveld refinement for polycrystalline X-ray diffraction at very affordable rates. Please contact our X-ray crystallographer if you are interested. You can find contact information below. Training sessions are also offered to students and academic users at reasonable rates.


Teaching and Training

A graduate course (CHEM 681) in X-ray Crystallography is offered in the department that covers a general introduction to X-ray diffraction with hands on experience in mounting crystals on the diffractometers, unit cell determination, data collection and processing, methods of solving crystal structures, refinements, analysis of derived results and preparation of materials for publication.
Graduate students and post-doctoral fellows in the department are encouraged to participate in training sessions for operating X-ray diffractometers. Hands-on training provides opportunities to characterize structural features of your own samples in the solid state.