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 Apex4 User Manual - written for the Purdue Bruker Quest instrument with a sealed tube molybdenum source and Photon-II detector
  • Purdue Apex4 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 and Apex4

• 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

• 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).

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