1,2,3-Dithiazolyl and 1,2,35-Dithiadiazolyl Radicals as Spin-Bearing ...

was placed in the freezer overnight. While a crystalline product was not obtained, a dark,
amorphous powder did precipitate from solution. This was also identified as the target
species and was also shown to be pure by elemental analysis.
Despite these efforts we were never able to obtain anything more than infrared
and EPR data for V-1, which were not enough to say that the target radical was actually
obtained. The remainder of this portion of the chapter will review the characterization
data obtained for each of the precursor salts and what data there is for V-1.
5.2.3 Infrared Spectroscopy
As the starting material V-2 is fairly complex and while the IR has been reported 5 it
is important to first examine this spectrum. The sulfur-nitrogen stretches of the 1,2,5-
TDA moiety likely correspond to the weak absorption at 1262 cm -1
as well as the
medium absorption bands at 918 and 566 cm -1 . The bands associated with the C-N double
bonds of this ring are likely those at 1486 and 1537 cm -1 . The N-H amine stretches are
not shown in Figure 5-1, but there are two strong, sharp absorptions at 3494 and 3389 cm -
1 as well as the NH 2 scissoring at 1606 cm -1 . While this is in the same region as C-C
aromatic stretches the relative intensity suggests that it is most likely from the amine.
The C-Cl stretch shows up at 857 cm -1 . Only the components of the structure that will
likely be useful for tracking the changes of the compound through the series of reactions
to be discussed have been included. The other peaks in the spectrum are likely those
associated with ring bending and similar C-C infrared modes that will likely not change
substantially and are therefore not worth intensive examination.
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