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

Compound Name: 4-(2′-pyrimidyl)-1,2,3,5-diselenadiazolyl
MW: 277.0 g/mol
Synthesis and Structure:
black blocks
Appearance:
Lit. and/or
notebook # and page:
DM06-36 p53
DM06-38 p56
First made on
date: Jan 19, 2010
Made by:
Dan J. MacDonald
Experimental Data: Solid triphenylantimony (2.0622 g, 5.8408 mmol) was added to a
128 slurry of [pymDSDA + ][Cl − ] (3.5902 g, 11.489 mmol) in 100 mL of acetonitrile and
refluxed for 1.5 h. The resulting black powder was filtered and washed with 3 × 20 mL of
acetonitrile and dried in vacuo. Crude yield: 2.9619 g (94% based on
[pymDSDA + ][Cl − ]). Crystals suitable for X-ray crystallography were obtained by
dynamic vacuum sublimation (10 −2 Torr) at 110 °C. The solution X-band EPR spectrum
(CH 2 Cl 2 , 295 K) consists of one broad, featureless absorption (spectral signal width of ca.
150 G), with g = 2.0382, consistent with similar DSDA radical species. In the solid state,
the magnetic susceptibility measurements reveal that the title compound is diamagnetic
as expected on the basis of the strongly dimerized structure described.
.FTIR (KBr): 3122(w), 3058(w), 3028(w), 3018(w), 2977(w), 2964(w), 1736(w),
1557(s), 1435(w), 1418(s), 1345(m), 1270(w), 1256(w), 1226(w), 1180(m), 1106(w),
989(w), 968(w), 893(w), 877(w), 825(m), 798(w), 736(s), 723(s), 646(s), 632(s), 469(w),
426(w), 416(w).
EA Anal. Calcd for C5H3N4Se2: C, 21.68; H, 1.09; N, 20.22. Found: C, 21.86; H, 1.31;
N, 20.05
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