Resources for Data Collection, Data Workup and Publication Writing

Submitting Samples

• Single Crystal XRD
• Powder/Muliticrystalline XRD
• X-ray Fluorescence

Data Collection Manuals and Standard Operating Procedures (SOPs)

• Bruker Quest Single Crystal Diffractometers
  
  • Purdue Apex5 User Manual - written for the Purdue Bruker Quest instrument with a sealed tube molybdenum source and Photon-II detector
  • Purdue Apex5 User Manual - written for the Purdue Bruker Quest instrument with a copper X-ray microsource and Photon-III C14 detector
  • Purdue Twinning Manual for Apex2 - also mostly still applicable for Apex3, 4 and 5

• Panalytical Empyrean Powder X-Ray Diffractometer
  • SOP - Changing the stage to the five-axis cradle
  • SOP - Using the Anton Paar HTK hot stage

• Panalytical Epsilon 4 X-Ray Fluorescence Spectrometer
  
  • SOP - Basic Standardless Data Collection ("Omnian")
  • Theory of XRF (Panalytical pamphlet)
  • XRF Consumables Catalogue 2016 (Panalytical)

• Nonius KappaCCD using COLLECT - instrument retired
• Rigaku Rapid using CrystalClear - instrument retired
  
  • Integrating data with HKL3000/HKL2000

Installing XRD Software on your own computer

• Please see or email Dr. Zeller for files, license codes and instructions.

Resources for publications, single crystal diffraction

• Checkcif (link to the IUCr checkcif page)
• Purdue instrument details and checkcif entries:
  • General cif items for Purdue instruments (with instructions)
  • CIF items for the copper radiation Bruker Quest Diffractometer (please check instrument for up to date settings)
  • CIF items for the molybdenum radiation Bruker Quest Diffractometer (please check instrument for up to date settings)
• FinalCif (link to the software download page): automatically populates cif entries from the raw data files. The by far easiest way to finalize cifs and make publication quality tables. Read the software documentation before using.
  
  • FinalCif table and report templates (default templates are built into the software):
    • A template with everything in
    • A template without the report text
    • Custom Purdue template (H-atom treatment needs manual editing)
    • Custom Purdue template (simplified H-atom treatment)

• In case you need tables from multiple CIF files at once, there is the small program multitable which generates such tables. Scroll down the page to download the executable of the Windows Graphical version. 
• Typical general procedure writeup for publications (specific for Purdue's single crystal diffractometers)
• Making high quality images and figures using Mercury. Step-by-step instructions for setting up CCDC's Mercury to create high quality Ortep-like figures for publications and presentations.
• Making Tables and Ortep plots using the IUCr publcif tools page
• Combining multiple cifs into one (link to the IUCr catCIF page)
• Acknowledgements: If your data were collected on one of Purdue's Bruker Quest diffractometers, please include the following lines in the acknowledgement section of your publication:

This material is based upon work supported by the National Science Foundation through the Major Research Instrumentation Program under Grant No. CHE 1625543. (Funding for the single crystal X-ray diffractometer).

We thank the College of Science, Purdue University, for support for X-ray detector upgrades through the 2020 Laboratory and University Core Facility Research Equipment Program.

Resources for publications, multicrystalline diffraction

• Typical general procedure writeup for publications: For powders and Rietveld analysis using the reflection-transmission stage (Bragg-Brentano) or the capillary spinner (Debye-Scherrer mode)

Resources for publications, X-ray fluorescence

• Typical general procedure writeup for publications when using the Purdue University Panalytical Epsilon4 X-ray Fluorescence Spectrometer (Omnian Procedure)

Single Crystal Structure Refinement

The SHELX Programs:

• The Shelx Homepage
• List of Shelxl instructions
• Shelxle (GUI for Shelxl) 

Single Crystal Data Validation

• Platon: Platon
• Platon download for Windows
• Checkcif
• The checkcif dictionary

Links to databases and other external resources (Purdue credentials or campus computers only)

• CSD - Cambridge Structural Database (Purdue users only): Please e-mail Dr. Zeller for license codes and installation instructions. Win, Mac or Linux.
• WebCSD - web based copy of the Cambridge Structural Database for organic crystal structures. Contact the crystallographer or the Chemistry Library if you would like to install a copy of the full data base (Purdue computers only).
• ICSD - web based copy of the Inorganic Crystal Structure Database for inorganic crystal structures.
• ICDD - the multicrystalline XRD database, formerly the "Powder Diffraction File". A copy is now available for Purdue users on the control computer of the Panalytical Empyrean X-ray diffractometer in Wetherill 101. Please contact Dr. Zeller (zeller4@purdue.edu) for access to the database.
• International Tables of Crystallography
• All Chemistry Library resources