Dissertation - Open Access
Doctor of Philosophy (PhD)
The structures of: 1) 2-piperidino-5-chlorornethyl-5-rnethyl-2- oxo-1, 3,2-dioxaphosphorinan; 2) 2-phenoxy-5-chloromethyl-5-methyl-2- oxo-1, 3,2-dioxaphosphorinan; 3) 2-p-bromophenoxy-5-chloromethyl-5- chloromethyl-5-methyl-2-oxo-1, 3, 2-dioxaphosphorinan have been resolved by x-ray single crystal studies. A Picker 4 circle diffractometer employing molybdenum x-rays and a zirconium filter was used to obtain accurate data. The space group of the first two compounds is P21/c while that of the third is Pca21. The lattice constants of the compounds are: 1) a = 10.035(8)Å, b = 6.503(4), c = 20.19(1), β = 96.8(3)°; 2) a = 6.237(3)Å, b = 11.437(5), c = 19.419(9), β = 109.95(3); and 3) a = 12.67(2)Å, b = 9.13(1), c = 11.89(1). Density measurements indicated 4 molecules per unit cell for all the compounds. The structures of the first two compounds were solved by the direct method of symbolic addition as the initial sign determining process. The bromine atom of the third compound was located from a Patterson map and the remaining atoms located by Fourier and least squares techniques. All nonhydrogen atoms were anisotropically refined. The final weighted R factors are: 0.033, 0.036, and 0.054. The unweighted R factors are: 0.054, 0.063, and 0.12. The amide derivative prefers the lone oxygen in the axial position while the phenoxy and p-bromo-phenoxy derivatives prefer it in the equatorial position.
Library of Congress Subject Headings
South Dakota State University
Wagner, Richard Earl, "Applications of New Methods of Structure Determination" (1973). Electronic Theses and Dissertations. 5505.