Crystallographic Structure Determination: An Experiment for Organic Analysis and Other Nontraditional Venues

Abstract

Single crystal diffraction analysis is a technique being increasingly utilized by non-specialists. To give students an introductory experience in this method, a one to two hour lecture and a three hour lab are described for use in courses such as organic analysis, biophysical chemistry, and instrumental methods. This class emphasizes the practical aspects of diffraction analysis, especially how routine structures are solved, how the results are prepared for publication as graphics and tables, and how reliable these results are. The student employ x-ray diffraction analysis software (i.e. SHELXTL) to solve the structures of compounds from supplied crystallographic data sets. Three data sets appropriate for this experiment are provided (i.e. for PhCH2-NH-CHPh-P(O)(OH)(OEt), (η6-1,4-C6H4(NH2)(NMe2))Cr(CO)3, and Pd(Ph2PCH2CH2PPh2)(S2C2(CN)2)) as is a link to a Youngstown State University Structure Center WEB page (i.e. http://www.as.ysu.edu/~adhunter/YSUSC/XRAYDPST/index.html) where additional properly formatted crystallographic data files may be downloaded.