Supplementary Material Available: Listings of analytical data for the complexes (Table SI) and structure factors (Table S2) for the nickel complex (12 pages). Ordering information is given on any current masthead page.
Abstract. S4N4.AsF 5, monoclinic, P2~/m, a = 5.593(1), b = 11.062(2), c = 7.682(1) A, fl = 109.10 (1) °, U = 449.2 (2) A 3, Dc = 2.62 Mg m -3 for Z = 2; R~ = 0.036 for 848 non-zero data. The structure of this compound is comparable to those of all the other 1:1 adducts of S4N 4, with the exception of the adduct S4N4.CuC1. The coordination of the AsF 5 group to one of the N atoms results in the opening of the SaN 4 cage structure to a puckered boat-shaped ring with the four S atoms in a plane.Introduction. During attempts to prepare cationic derivatives of 84N4, the reactions of S4N 4 with the compounds Ss(AsF6) 2 and Ses(AsF6) 2 in SO 2 have been observed to give the species S6N4(AsF6) 2 and its selenium analogue Se4S2N4(AsF6)2 (GiUespie, Kent & Sawyer, 1980). However, when the corresponding reactions of S4N 4 with both Te4(AsF6) 2 in SO 2 and Ses(AsF6) 2 in methylene chloride were attempted, they gave a deep-red crystalline product which has been characterized by X-ray crystallography as a 1:1 adduct of S4N 4 with the Lewis acid AsF 5.Crystals of S4N 4. ~sF 5 exist in a variety of forms depending on the reaction conditions. An approximately spherical crystal of this material was selected from the product of the reaction of Sea(AsF6) 2 with S4N 4 and sealed in a Lindemann capillary. Accurate unit-cell dimensions were obtained by least-squares refinement with 15 high-angle reflections measured on a Syntex P2~ diffractometer using Mo Ka radiation.(2 = 0.71069 A). Data were originally collected to a maximum 20 of 50 ° using a B-centred cell a' = 5.593, b'= 11.062, c'= 14.561 A withfl' = 92.33 ° and later transferred to the primitive cell above. Reflections were measured using 0-20 scans over a 20 scan range (Ka~ -0.9 °) to (Ka 2 + 0.9 °) and variable scan rates of 4-29.3 ° min -~ depending on the intensity of preliminary count. A total of 2260 data in the
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