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Chemistry 5832: Solid State Structural Methods, Winter 2004
Laboratory Assignment #2 - Introduction to SHELXTL
Individual Project
Getting Used to the Basics of SHELXTL to Solve Structures. On the computer, there are three selected X-ray data sets (i.e. Fun1 {PhCH2-NH-CHPh-P(O)(OH)(OEt)}, Fun2 {(h6-1,4-C6H4(NH2)(NMe2))Cr(CO)3}, and Fun3 {(Ph2PCH2CH2PPh2)Pd(S2C2(CN)2)}) chosen based on the variety of their structures and the fact that their structure solutions proceed in a relatively strait forward fashion. For each of these examples, copy its data from the directory where it is currently located to your directory and then make a backup copy.
(1) Run the program XS on your data to find a trial solution from which you can guess the first atom(s).
(2) Run the program XP to display this trial solution and assign any atoms who’s identities are unambiguous.
(3) Run the program XL to refine the data and obtain a better solution for the crystal structure.
(4) Repeat steps 2 and 3 until you have completely assigned and refined the structure. [Note: after you have assigned and refined all non-hydrogen atoms convert the refinement model to anisotropic (ANIS), then do an extinction correction (EXTI), and add the ACTA (BOND $H) command. Then assign any hydrogen atoms and refine them. Finally, refine the data until the solutions stops improving (these last three commands are added to the *.ins file using the DOS edit command).]
(5) Print at a final view of your molecule using XSHELL and hand in this material. Save your .ins files on disk for the three structures as we will come back to them later.
Some common XP commands are:[1]
fmol Loads the data into XP
info Shows the tabular data for the molecule
proj Shows a 3D view of the molecule
pick Allows you to assign atoms
kill Allows you to kill atoms
bang Shows a list of bond lengths and angles
file Saves your results
exit Exits from XP
D:\1 ADH Data Files\Teaching\5832 Solid State Structural Methods\5832 Winter 2004\Chemistry 5832 Lab Exercises\Chemistry5832.LabExercise.2.SHELXTL-1.Winter2004.048a.doc
[1] Detailed explanations of all of these commands and more details on using the SHELXTL software are found in the manual “X-Ray Structure Solution via SHELXTL: A Beginner’s Introduction” available in the X-ray lab and as a .pdf file on my web site at: http://www.as.ysu.edu/~adhunter/Teaching/Chem5832/index.html