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Molecular Structure Laboratory


Molecular Structure Laboratory / Policies Updated: October 26, 2015

  • Sample Submission
  • Instrument Access
  • Instrument Operation Instructions
  • Charges and Fees
  • Co-authorship Policy

Sample Submission

Single-Crystal: All users are required to fill out the first page of the submission form and submit one form per sample. The submission form is available in two formats, SubmissionForm.docx and SubmissionForm.pdf. Please print out both pages; a double-sided copy is preferred. A supply of submission forms can be found on the sample submission table in the X-ray Lab (2121 Chemistry). We can handle dry, air- and moisture-sensitive, and solvent-dependent crystals. If you are not sure how sensitive your crystals are - handle them as air-sensitive and submit them in mother liquor. If you wish to get your sample back clearly indicate that on the submission form. For specific questions or concerns regarding your sample you may contact Director of X-ray Laboratory by e-mail or in person. To submit a specimen by mail follow the steps on the Submit a sample page.

Powder Diffraction: Users are responsible for preparing their samples. Sample holders and related equipment is available at the Powder diffraction lab (room 2143).

Instrument Access

Single-crystal: the instruments are reserved on the first come first serve basis. If the sample needs to be characterized urgently an exception can be made, in which case you ought to contact Ilia Guzei. The submission form should be placed on the submission table in the X-ray laboratory. If you wish to discuss your sample in person you are welcome to talk to Dr. Ilia Guzei or X-ray TA Brian Dolinar.

Powder diffractometer: trained users may sign up at http://xray-calendar.chem.wisc.edu for 15-minute time slots with no more than three consecutive time slots at a time. Extended data acquisitions may be run between 6:00 PM - 8:00 AM and on the weekends. First timers: you should contact Ilia Guzei for instrument/software training and sign up for a mutually convenient 45-minute time period.

Instrument Operation Instructions

Users planning to use the powder diffractometer should familiarize themselves with the Diffractometer Operation Notes and EVA Instructions.

Single Crystal X-ray Diffraction Experiment through the eyes of Dr. Maik Tretbar (Schomaker Laboratory) - a PowerPoint presentation.

Charges and Fees for Single-Crystal and Powder analyses

For single-crystal analysis:

As of July 1, 2011, the following charges have been instituted for academia users:

  • Unit cell determination - $ 20.00.
  • Partial data set with a structural solution - $ 100.00.
  • A complete dataset acquisition only (without structural solution and refinement) - $ 100.00.
  • A complete structural characterization (also see Co-authorship Policy) - $ 220.00.
  • A room temperature powder pattern - $20.00 (This is not done routinely and should be discussed beforehand).

For all datasets acquired at low temperature the cost of liquid nitrogen is billed directly to the group. For the academic out-of-house customers the cost of the liquid nitrogen is $15.

The university overhead (50%) and the departmental overhead (6%) are added to all charges.

Industrial users - contact Director of X-ray Laboratory.

For powder diffraction: contact Director of X-ray Laboratory.

For the 2012 hourly rate contact the Lab Director. In 2012 the instrument access is limited to the members of the Chemistry Department.

Co-authorship Policy

Co-authorship guidelines that will be followed at the Molecular Structure Laboratory are in accord with ACA regulations and with co-authorship policies accepted at the majority of crystallographic laboratories.

If the structural information is a major part of the intellectual content of the paper, and if this information has been derived primarily by X-ray diffraction, then the crystallography should be included in the paper and the crystallographer should be considered for co-authorship. Most papers that include metric parameters (i.e. distances and angles), ORTEP diagrams, and structural discussions would fall under this classification. I am encouraging collaborators to use my expertise in structural discussion (packing, hydrogen bonds, inter/intramolecular contacts, etc.), structure comparison, and database searching for relevant compounds. I will also assist in the preparation of, and review manuscripts that include my structural data. I would like the opportunity to review all papers that include structures solved by me before they are sent off for publication.

If crystallography is used only to confirm a structure that is well established by other means (NMR, mass spec, etc.), and if no structural details are given in the paper, only an acknowledgment is more appropriate. This would occur, for example, when the relative stereochemistry of an intermediate in a complex organic synthesis has been determined, or when the crystallographic experiment was routine and structural determination was straightforward. In such cases, the crystallographer would be willing to publish the structural results of the investigation in a crystallographic journal upon mutual agreement. An acknowledgement may also suffice in the cases when the X-ray experiment was standard and the structure solution straightforward.

The guidelines above are intended to help authors prepare manuscripts, facilitate their publication, and to protect the authors of manuscripts from errors in professional presentation of crystallographic results.

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