Preparation, X-ray Structure, and Spectroscopic Characterization of 1,5-Se₂S₂N₄

Abstract

The reaction of [(Me(3)Si)(2)N](2)S with equimolar amounts of SCl(2) and SO(2)Cl(2) produces S(4)N(4) in a good yield. The new chalcogen nitride 1,5-Se(2)S(2)N(4) has been prepared in high yield by two different reactions: (a) from [(Me(3)Si)(2)N](2)S and SeCl(4) and (b) from [(Me(3)Si)(2)N](2)Se with equimolar amounts of SCl(2) and SO(2)Cl(2). 1,5-Se(2)S(2)N(4) has a cage structure similar to those of S(4)N(4) and Se(4)N(4). The crystal structure is disordered with site occupation factors ca. 50% for selenium in each chalcogen atom position. The 12 eV EI mass spectrum shows Se(2)SN(2)(+) as the fragment with highest mass. Both the (14)N and (77)Se NMR spectra show a single resonance (-238 and 1418 ppm, respectively). These data rule out the possibility that the crystalline sample is a solid solution of S(4)N(4) and Se(4)N(4) and imply the presence of 1,5-Se(2)S(2)N(4). This deduction was further verified by Raman spectroscopy and vibrational analysis.

Tellurium: a maverick among the chalcogens

“…39 These dications may be viewed as either (a) phosphine-stabilised Te 3 2+ dications (36a) or (b) complexes of the Te 2+ dication with two TePR 3 ligands (36b) (Scheme 14). 41 Although TeCl 2 is only available as an in situ reagent generated by reduction of TeCl 4 with Me 3 SiSiMe 3 , the adduct tmtuÁTeCl 2 (tmtu = tetramethylthiourea) is well-known and has been used in metathetical reactions (ref. Several complexes of the Te 2+ dication with monodentate electrondonor ligands, e.g.…”

“…46 Interestingly, halogenation of ditellurides with less bulky aryl substituents generates mixed-valent ditellurium dihalides ArX 2 Te IV -Te II Ar (Ar = 2,6-dimesitylphenyl) (Section 1). PPh 3 (41), NHC (42) (Scheme 18), 46,47 or via [1+4] cycloaddition with 2,3-dimethyl-1,3-butadiene. PPh 3 (41), NHC (42) (Scheme 18), 46,47 or via [1+4] cycloaddition with 2,3-dimethyl-1,3-butadiene.…”

The Nature of Transannular Interactions in E4N4 and E82+ (E = S, Se)

“…1 Tetrasulfur tetranitride (1a) is an archetypical member of this group: 2 S4N4 has a cage-like structure with two short intramolecular S⋯S interactions as determined by single crystal X-ray diffraction ( Figure 1). [3][4][5] The selenium analogue of 1a is also known (1b), [6][7][8] as is the hybrid species S2Se2N4 (1c), 9 and they are both structurally isomorphous with S4N4.…”

Preparation and X-Ray Structure of 4-N,N′-Bis(trimethylsilyl)- amino-3,5-diisopropylphenylselenium Trichloride

“…The reactions o f selenium halides, in particular SeC l2, w ith prim ary am ines are being investigated in our laboratories [1]. The preparation o f cyclic or linear selenium im ides is one goal o f this re search.…”