Magnetization, heat capacity, and neutron diffraction experiments on t
he beta-phase of the dithiadiazolyl radical, p-NC.C6F4.CNSSN., provide
conclusive evidence that this system exhibits noncollinear antiferrom
agnetism at 35.5 K, an unprecedented temperature for an organic radica
l. On the basis of magnetization and powder neutron diffraction result
s, coupled with theoretical calculations of the spin distribution with
in the molecule, a magnetic structure for this compound is proposed in
which the interactions propagate through S ... N contacts.