3‐Diethylamino‐5‐phenyl‐1,2,4‐diselenazolium‐tetrachloroniccolat(II) — Synthese und Struktur

Abstract

Inhaltsiibersicht.Bis-(N ' , N ' -diethyl-N-benzoylsele-interpretiert werden. Die Verbindung besteht aus noureato)nickel(II) reagiert mit Diphosgen in Benzen 1,2,4-Diselenazolium-Kationen, die als planare Fiinfzu 3-Diethylamino-5-phenyl-l , 2,4-diselenazolium-tetra-ringe vorliegen und aus tetraedrischen Tetrachloroniccochloroniccolat(II), dessen Rontgenkristallstrukturanalyse lat(I1)-Anionen. Sie ist zu 3-Diethylamino-5-pheund Rontgenphotoelektronenspektrum vorgestellt und nyl-1 ,2,4-dithiazolium-tetrachloroniccolat(II) isomorph. 3-Diethylamino-5-phenyl-l,2,4-diselenazolium-tetrachloroniccolate(II) -Synthesis and StructureAbstract.Bis-(N ' , N ' -diethyl-N-benzoylselenourea-3-diethylamino-5-phenyl-l , 2,4-dithiazolium-tetrachloroto)nickel(II) reacts with diphosgene in benzene to niccolate(I1).3-diethylamino-5-phenyl-1 , 2,4-diselenazolium-tetrachloroniccolate(I1). Its structure is confirmed by RKSA and ESCA. The compound consists of cations, which are planar fivemembered rings and of tetrahedral tetrachloroniccolate(I1) anions. The complex is isomorphic with selenaheterocyclic cation; synthesis; crystal structure

Intra- and intermolecular Se...X (X = Se, O) interactions in selenium-containing heterocycles: 3-benzoylimino-5-(morpholin-4-yl)-1,2,4-diselenazole

“…The bond lengths within the 1,2,4-diselenazole ring (Table 2) are comparable with those in 3-dimethylamino-5-phenyl-1,2,4diselenazolium tetrachloroniccolate (Rosenbaum et al, 1992), although the Se-Se bond in (I) is about 0.09 Å longer than that in the earlier report [2.293 (1) Å ]. There are no other structures containing an unfused 1,2,4-diselenazole ring recorded in the Cambridge Structural Database (CSD, Version 5.35 of 2013 plus two updates; Allen, 2002), although a structure incorporating a 1,2,4-diselenazolidine ring (all bonds in the ring are saturated; Takikawa et al, 1995Takikawa et al, , 2006 has an Se-Se distance of 2.331 (2) Å , while the Se-C and C-N bonds are about 0.15 and 0.07 Å longer, respectively, than those in the 1,2,4-diselenazoles.…”

“…The structure of the latter, containing fused 1,2,4-diselenazole rings with a tetravalent Se atom, was established by X-ray crystallography (Richter et al, 1991). In contrast with the corresponding sulfur analogues, 1,2,4-diselenazole derivatives have rarely been described (Burger & Ottlinger, 1978;Liebscher et al, 1979;Shibuya, 1986Shibuya, , 1987Rosenbaum et al, 1992). In the case of 3-dimethylamino-5-phenyl-1,2,4-diselenazolium tetrachloroniccolate, a crystal structure is available (Rosenbaum et al, 1992).…”

“…In contrast with the corresponding sulfur analogues, 1,2,4-diselenazole derivatives have rarely been described (Burger & Ottlinger, 1978;Liebscher et al, 1979;Shibuya, 1986Shibuya, , 1987Rosenbaum et al, 1992). In the case of 3-dimethylamino-5-phenyl-1,2,4-diselenazolium tetrachloroniccolate, a crystal structure is available (Rosenbaum et al, 1992). The title compound, (I), was obtained unexpectedly as an uncharacterized side-product.…”

Acylselenoureas, selenosemicarbazones and selenocarbamate esters: Versatile ligands in coordination chemistry

“…The Ni (II) complex [Ni{PhC(O)NC(Se)NEt 2 } 2 ] reacts with diphosgene in benzene to afford a heterocyclic diselenazolium salt (Scheme 3), which was structurally characterised. 59 Scheme 3…”

Product Class 27: Selenazoles and Tellurazoles Containing One or More Other Heteroatoms

“…[18,19] 13.27. [17] Scheme 18 Synthesis of the Nickel Complex of a 1,2,4-Diselenazolium Salt [17] Bis[3-(diethylamino)-5-phenyl-1,2,4-diselenazolium] Tetrachloronickelate Complex (35): [17] A soln of bis(N-benzoyl-N¢,N¢-diethylselenoureato)nickel (34; 16.5 g, 27 mmol) in petroleum ether (130 mL) was stirred at rt while a soln of trichloromethyl chloroformate (5.35 g, 27 mmol) in petroleum ether (30 mL) was added dropwise over 30 min. When it is treated with sodium hydrogen selenide, the diselenobiuret which is formed can be oxidatively cyclized to afford the diselenazolium salt 33 (Scheme 17).…”