0000000000517042
AUTHOR
Arto Maaninen
Preparation and structural characterization of (Me(3)SiNSN)(2)Se, a new synthon for sulfur-selenium nitrides.
The reaction of (Me(3)SiN)(2)S with SeCl(2) (2:1 ratio) in CH(2)Cl(2) at -70 degrees C provides a route to the novel mixed selenium-sulfur-nitrogen compound (Me(3)SiNSN)(2)Se (1). Crystals of 1 are monoclinic and belong the space group P2(1)/c, with a = 7.236(1) A, b = 19.260(4) A, c = 11.436(2) A, beta = 92.05(3) degrees, V = 1592.7(5) A(3), Z = 4, and T = -155(2) degrees C. The NSNSeNSN chain in 1 consists of Se-N single bonds (1.844(3) A) and S=N double bonds (1.521(3)-1.548(3) A) with syn and anti geometry at the N=S=N units. The N-Se-N bond angle is 91.8(1) degrees. The EI mass spectrum shows a molecular ion with good agreement between the observed and calculated isotopic distributions…
Halogenation of tellurium by SO2Cl2. Formation and crystal structures of (H3O)[Te3Cl13]·1/2SO2, [(C4H8O)2H][TeCl5]·(C4H8O), [(Me2SO)2H]2[TeCl6], and [Ni(NCCH3)6][Te2Cl10]
Abstract The halogenation of elemental tellurium with SO2Cl2 in various solvents has been investigated. (H3O)[Te3Cl13]·1/2SO2 (1) and [(C4H8O)2H][TeCl5]·(C4H8O) (2) were obtained in CS2 and THF, respectively. When DMSO is added into the THF solution of tellurium and SO2Cl2, [(Me2SO)2H]2[TeCl6] (3) is formed. In the acetonitrile solution tellurium and SO2Cl2 form [Ni(NCCH3)6][Te2Cl10] (4) in the presence of metallic nickel. All compounds 1–4 were characterized by 125Te NMR and by X-ray crystallography. The formation of the anions has been discussed.
ChemInform Abstract: Preparation and Structural Characterization of (Me3SiNSN)2Se, a New Synthon for Sulfur-Selenium Nitrides.
The reaction of (Me(3)SiN)(2)S with SeCl(2) (2:1 ratio) in CH(2)Cl(2) at -70 degrees C provides a route to the novel mixed selenium-sulfur-nitrogen compound (Me(3)SiNSN)(2)Se (1). Crystals of 1 are monoclinic and belong the space group P2(1)/c, with a = 7.236(1) A, b = 19.260(4) A, c = 11.436(2) A, beta = 92.05(3) degrees, V = 1592.7(5) A(3), Z = 4, and T = -155(2) degrees C. The NSNSeNSN chain in 1 consists of Se-N single bonds (1.844(3) A) and S=N double bonds (1.521(3)-1.548(3) A) with syn and anti geometry at the N=S=N units. The N-Se-N bond angle is 91.8(1) degrees. The EI mass spectrum shows a molecular ion with good agreement between the observed and calculated isotopic distributions…