Data Collection on the Nonius Kappa CCD Diffractometer

This is a sort of walk-through guide - a checklist of things to do during data collection and processing. If you are a novice you may need to refer to each section in detail as you proceed. As you gain experience, much of this should become second nature. There is no reason why any self-respecting synthetic chemist should not be able to produce crystallographic results that withstand peer review.  All you need is to do it correctly.

The descriptions that follow may seem detailed but they barely scratch the surface of describing the situations that you may encounter.  These pages are neither definitive nor exhaustive - they can't cover everything. They cover much of what you need to know to be successful with a routine crystal, but not much else.

You should be prepared to seek professional help, experiment, add detail and even use your brain. Many crystals are not routine, but that does not necessarily mean they are difficult. Other crystals appear to be routine but are not. Be aware that the KappaCCD is capable of dealing with crystals that would have been rejected in most laboratories just a few years ago.

1) Make sure the low temperature machine is running. 

2) Check that the x-rays are on and turned up to 50kV; 30mA.

3) Prepare the diffractometer for mounting.

4) Find or make a mounting pin.

5) Prepare to mount a crystal.

6) Choose the most suitable crystal.

7) Mount the crystal on the diffractometer.

8) Centre the crystal on the diffractometer.

9) Inspect the crystal.

10) Index the crystal

11) Orient the crystal, identify and index the crystal faces (usually optional).

12) Determine the resolution limit of diffraction.

13) Prepare a set of data collection scans.

14) Start your data collection.

Return to the main Tutorials page or to the main X-Ray Lab page