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

y flash distillation, and the residue was divided into two portions, each of which was
sublimed under a dynamic vacuum at 120 °C (10 −2 Torr), yielding dark-blue needles of
II-8 (0.2543 g; 27% yield based on Znhfac 2·2THF) suitable for X-ray crystallography
and magnetic measurements. ν max (KBr)/cm −1 : 3138(w), 2961(w), 2914(w), 2851(w),
1647(s), 1586(w), 1560(m), 1532(m), 1487(s), 1463(m), 1389(m), 1348(w), 1319(w),
1259(s), 1208(s), 1150(s), 1137(s), 1097(m), 861(w), 841(w), 813(m), 796(m), 763(w),
743(w), 716(w), 669(m), 647(w), 586(m), 526(w). Anal. Calcd. for
C 55 H 17 F 48 Zn 4 N 12 O 16 S 6 : C, 26.76; H, 0.69; N, 6.81%. Found: C, 27.12; H, 0.89; N, 6.75%.
X-ray: P 2 1 /n, a = 19.884, b = 8.8599, c = 23.216, β = 100.73, R = 5.09.
2.7 References
(1) Preuss, K. E. Dalton Trans. 2007, 2357.
(2) Wu, J.; MacDonald, D. J.; Clérac, R.; Jeon Ie, R.; Jennings, M.; Lough, A. J.;
Britten, J.; Robertson, C.; Dube, P. A.; Preuss, K. E. Inorg. Chem. 2012, 51, 3827.
(3) Jennings, M.; Preuss, K. E.; Wu, J. Chem. Commun. 2006, 341.
(4) Cordes, A. W.; Bryan, C. D.; Davis, W. M.; Delaat, R. H.; Glarum, S. H.;
Goddard, J. D.; Haddon, R. C.; Hicks, R. G.; Kennepohl, D. K.; Oakley, R. T.; Scott, S.
R.; Westwood, N. P. C. J. Am. Chem. Soc. 1993, 115, 7232.
(5) Cordes, A. W.; Glarum, S. H.; Haddon, R. C.; Hallford, R.; Hicks, R. G.;
Kennepohl, D. K.; Oakley, R. T.; Palstra, T. T. M.; Scott, S. R. Chem. Commun. 1992,
1265.
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