The Crystallography Center at Purdue is located in room 234 of the Weatherall Chemistry Building. The lab is designed to provide structural data from single crystal diffraction studies. The phone number is (765) 494-4572.
Lab Hours
Mon -- Fri 9 a.m.-- 4 pm
The new RAPID Diffractometer is UP!
There is no low temperature yet. Hopefully it will be installed no later than February 17.
The old KappaCCD should be able to collect data by the middle of next week.
The 2009 version of CSD is here. You can get dvd disks for windows, mac and linux from the x-ray lab.
The center is run by Dr.
Phillip Fanwick. He
is an experienced crystallographer having over 500
publications
and has extensive 
experience in both organic
and inorganic small molecule crystallography.
It is his job to collect the data, solve the structure, and provide
a report suitable for publication. He is also available for
consultation
with regards to growing crystals, interpretation of data, and other
aspects
of structural studies. In addition computer programs can be
written
to facilitate interpretation of the data and communication
between program packages.
The laboratory is set up to provide quick results. Usually there is minimal backlog and results are typically provided within 48 hours of sample submission. The current charge is $350 per structure for academic users and about $1140 for commercial samples.
The lab is located in room 234 of the Wetherall Chemistry Building and can be reached at (765)494-4572.
The lab is equipped with state of the art equipment.
1. A Nonius KappaCCD diffractometer mounted on a high intensity FR571 rotating anode x-ray generator. This is one of the few CCD/rotating anode systems in the world used exclusively for small molecule crystallography. Currently inoperative.
2. A Nonius CAD-4 diffractometer on a sealed tube copper x-ray source. Currently inoperative.
3. An Oxford Cryosystems low temperature device capable of temperatures from 400 to 90 K.
4. LINUX pc's used for structural calculations and the Cambridge Structural Database.
5. Other computers needed for collecting and processing diffraction data
You can get a real time view of the current laboratory activity here!
Note the screen in the upper right hand corner provides information about the current lab activity:
IDLE-- the diffractometer is idle
DOWN--the diffractometer is not working
CLOSED--the lab is closed because the crystallographer is not at work
PUMP--the rotating anode is establishing the required high vacuum
Sample name--id of sample currently collecting data
Laboratory Operations
In general the Crystallography Lab is open from about 9 to 4 Monday through Friday. It is suggested you check the lab view page (click above) to make sure the lab has lights on before heading over.
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 charge for an extra hour of useage ($50 for in-house users and about $200 for commercial users)! Useful advice on growing crystals suitable for crystallographic studies can be found on the useful links page. Typically data are collected at 150K as this produces the best and sharpest data. Data collection at room temperature should be requested only if there is a need to use this temperature. If there is any chance that the structure will be published in Acta Crystallographica then the box indicating this should be checked. Only the highest grade of crystals will be accepted if this box is checked. If you do not indicate your intent to publish there and then later submit to this journal there is a high likelihood the structure will not meet their very stringent requirements. Off campus users can mail samples to:
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.
The lab is a member of the Reciprocal Net Project. The Reciprocal Net at Purdue can be reached at
http://xraylab.chem.purdue.edu
News from the lab can be found here.