The complex (Et4N )[Fe(SPh)2(NO)2] (2) has been obtained as black crystals by treatment of K[Fe4S3(NO)7]·H2O with potassium hydroxide in molten diphenyldisulfide and subsequent addition of methanol and tetraethylammonium chloride. 2 is orthorhombic, space group Pbca, Z = 8, with a = 18.853(3), b = 17.958(3), and c = 13.283(2) Å at 140 K. The X-ray structure of 2 has been refined to R1 (R2) = 2.7% (3.1% ). It reveals a pseudotetrahedral S2N2 arrangement around the iron atom (Fe -S 2.280, Fe -N 1.679 Å (mean values), S -Fe -S 109.73(2)°, N -Fe -N 117.36(9)°) and Fe -N -O groups of the linear type (N -O 1.180 Å , Fe -N - O 169.0° (mean values)). The N - O bond order is 2.2. Structural properties as well as the low Mößbauer isomeric shift ( + 0.08 mm/s relative to Fe metal) are indicative of strong Fe - N π-back bonding and a major contribution of the mesomeric form Fe = N = Ō̱
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