Automating the Single Crystal XRay Diffraction Experiment Mark

Automating the Single Crystal X-Ray Diffraction Experiment Mark E Light School of Chemistry University of Southampton, UK Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

Presentation Outline Reasons for automation Requirements for an automated system Main challenges in building such a system Work flow to clearly define the problem Building and linking of system components Inline evaluation Software development Output of results Ongoing and future developments Animations Acknowledgments Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

Why Automate? General reasons for building an automated system: Maximise instrument usage – can do lots of shorter collections overnight Prioritise crystallographers time – let the robot do the tedious work Utilise the ‘data fit for purpose’ ideas Allows easy screening of many samples Ideal for polymorphism studies Allows for remote access Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

Requirements for an Automated System Once started should not need human intervention Ability to reliably place the crystal in the beam Obtain sensible unit cell Reject poor samples Automatically setup and perform data collection Make sensible decisions about exposure time, frame angle etc Allow configuration but with robust defaults Run unattended in a safe manner Clearly report progress and status Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

Main Challenges 1. 2. 3. 4. 5. Automatic changing of the sample Hands free crystal centring Automation of the data collection Continual Inline evaluation Development of a graphical control interface These can be placed within the following work flow Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

Setup via GUI Control Flow Sample Tray Bru. No Unmount Bru. No Mount Pre. Scans Diffraction No Yes Unit Cell Success No Yes Strategy Data Collection Data Process System Y Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

1. Sample Changing Mitsubishi Movemaster RV 1 A 6 axis industrial robot with a CR 1 controller – 30 K Internal control program accessed via serial port 24 capacity sample tray – bolted to table Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

2. Crystal Centring Uses accurately constructed pips Specially designed goniometer head employed Largest collimator used to maximise beam size at crystal (0. 6 mm) Some miscentring is allowable Why not use motorised goniometer head and image recognition software? Considerable added cost Added system complexity Additional sample runtime Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

3. Automated Data Collection As defined in the work flow – the following steps are carried out Determination of crystal diffraction characteristics – using prescans evaluate Determination of unit cell using phi/chi scans and Dir. Ax - evaluate Carrying out of strategy calculation and data collection Processing of data Running of structure solution and refinement - validate Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

5. Control GUI Requirements Data Collection: Well structured logic flow and failsafe error handling Sensible automated parameter choices GUI Easy sample selection and meta data input Highly configurable but with robust defaults Clear progress status Developed X-Tray Written in python using tkinter and the Bruker-Nonius Collect package. Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

X-Tray sample setup Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

X-Tray experiment setup Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

X-Tray experiment monitoring Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

Output of Results For an automated experiment the ultimate aim is a completed structure! Intermediate results are presented to the user: html report containing full experiment details hkl reflection file Starting point shelx instructions file to present to user or System-Y System-S best try at structure System-Y results Structure validation report Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004

Ongoing and Future Developments Improvements to the pip manufacture Improvements to the goniometer head Completion of the collision safety circuit Inline ranking of samples – so that poor samples are evaluated and then put at the back of the queue Addition of a controlled environment for queued samples Improved unit cell evaluation Develop results dissemination Automating the Single Crystal X-Ray Diffraction Experiment – Mark Light – School of Chemistry - University of Southampton – ECM 22 – Budapest 2004