Data collection, structure analysis, and crystallography consulatation services.

Lab News

    The 2010-2011 CSD is here.  Come to the lab to get a copy.

Sample Submission

Samples must be submitted by completing the on line submittal form.   All items in yellow must be filled in.  Incorrectly completed forms will be rejected.  The form may also be completed in the lab.  In this case, make sure the account to be billed and the formula are known. Samples submitted without a formula or with misleading information will be charged for a consulting fee of ($68.57/hr for in-house users and about $105.60/hr for commercial users)!

Samples may be left on the desk on the right as you enter the lab.  Make sure the sample is labeled with the compound id from the submittal form!  Either the structure should be provided on the printed submittal form or as a separate page when the sample is brought to the lab.  The form must be signed at this time.   Samples can be left next door in WTHR 236 if the lab is closed.  Samples are NOT run in order of submittal but based on the size and quality of the crystals and the research group's use of the lab.  In general, the equipment will not be reserved for use at a set time and samples must be left in the lab.  Air sensitive samples may be sealed in glass tubes or submitted coated with mineral oil or paratone.  Samples which lose solvent maybe submitted in their mother liquor.  A refrigerator and freezer are available for storing thermally sensitive crystals.   If it is desired that a sample be mounted as soon as it is brought to the lab then it should be brought down first thing in the morning!

The sample is analyzed several ways before data collection.  First, it is studied under a polarizing microscope.  This is a good test of crystal quality.  It is also determined if they are large enough to allow for data collection.  If the sample appears to have a chance of success, it is mounted and examined on the diffractometer.  A quick scan is made to determine if the quality is good and size are sufficient.  If the crystals fail any of the above inspections, the sample is rejected and there is no cost to the user.  Next, the unit cell is determined.  If the cell size strongly suggests the sample is not the intended compound it is rejected.  Also the Cambridge Structural Database is searched to see if the cell corresponds to a known structure.  Once the cell is indexed there is a charge of $50 to in-house users and about $200 to commercial users.  If the crystal passes all the preliminary checks, a data set is collected.  Rarely, the data does not lead to a structure.  In those cases there is no charge.

When the sample has progressed as far as possible, the user will be notified by e-mail.  If the structure was completed then the results will be found next to the submittal box in the lab.  Only a CD containing the raw data, Shelx files, and various tables in RTF format is provided.  A view of the molecule and labeling can be obtained from the Reciprocal Net site below. Users need an account and password to access their structures on the web.  It is the users responsibility to produce graphics for publication, print any tables and edit and submit the cif file.  Information about various freely available graphics programs for pc's is available here.  Also included is the program ENCIFR for editing CIF files for publication.

Staff

Equipment

Recent Publications

Lab submittal form

Crystallography course

Useful Links:

Crystallography Lab at North Carolina State University
(great discussion on growing crystals)

The University of Wisconsin (growing crystals)

CCP14
(the all purpose crystallographic site. Information on all aspects of crystallography with many references to software.)

International Union of Crystallography

American Crystallographic Association