Jürgen Hartung

Crystal Structure of Bis(3-Diethylamino-5-phenyl-1,2,4-dithiazolium) Hexachlorodicuprate, (dpd)2Cu2Cl6, at 120 K.

Abstract The crystal structure of the compound (dpd)2Cu2Cl6 at 120 K has been determined. Space group P21 /n , Z = 2, 3997 collected reflections, R = 6.8. Lattice dimensions (120(1)K) : a = 7.328 (8), b = 16.863 (14), c = 13.271 (10) Ä; β = 91.44(7).

Notizen: 3-Diethylamino-5-phenyl-1,2,4-dithiazolium-hexachlorodicuprat(II) und -tetrachlorocuprat(II), (dpd)2Cu2Cl6 und (dpd)2CuCl4 / 3-Diethylamino-5-phenyl-1,2,4-dithiazolium Hexachlorodicuprates(II) and Tetrachlorocuprates(II), (dpd)2Cu2Cl6 and (dpd)2CuCl4

(dpd)2Cu2Cl6 has been prepared by the reaction of bis(1,1-diethyl-3-benzoyl-thioureato)-copper(II) with SOCl2 in nitromethane. The brown air stable crystals were characterized by X-ray structure determination. Space group P21/n, Z = 4, 4222 observed unique reflexions, R = 0.053, Lattice dimensions (22 °C): a = 1336.4(2), b = 1677.2(9), c = 749.3(2) pm; β = 92.46(2)°. Similar reaction in acetonitrile yields stable orange crystals of (dpd)2CuCl4.

Substituierte 1,2,4-Thiadiazolium-dichloroaurate(I) und -tetra- chloroaurate(III) als Reaktionsprodukte von N-Thiocarbamoyl- benzamidinen mit TetrachIorogold(III)-Verbindungen / Substituted 1,2,4-Thiadiazolium dichloroaurates(I) and -tetrachloroaurates(III) as Products o f the Reaction o f N -Thiocarbam oyl-benzamidines with Tetrachlorogold(III) Compounds

Abstract The reactions of N-diethylaminothiocarbonyl-benzamidines Et2N-C(S)-N=C(NHR)-Ph (1: R = Ph, 2: R = C3H7, 3: R = H) with gold(III) compounds were studied. Treatment of 1 and 2 with equivalent amounts of tetrachlorogold acid gives 2,3-substituted 5-diethylamino-1,2,4- thiadiazoliumdichloroaurates(I) (1a, 2a). With tetrachlorogold acid in excess 1 yields 2,3-diphenyl- 5-diethylamino-l,2,4-thiadiazolium-tetrachloroaurate(III) 1b. With 3 and Na[AuCl4] bis(3-phenyl-5- diethylamino-1,2,4-thiadiazolium)-chloride-tetrachloroaurate(III) 3b is produced. The structures of la, 2a and 3b were investigated by X-ray structure analysis. In la and 2a the dichloroaurate(I) ions are linear. In the 1,2,4-thiadiazolium cations the N-C-bond lengths alternate characteristically. In 3b the tetrachloroaurate(III) ion is square planar. The 1,2,4-thiadiazolium cation shows a different alternation of N-C bond lengths in comparison with la and 2a which suggests changes in the thiadiazolium ring in 3b to a tautomeric form as confirmed by the localization of the H atom at the N atom in ring position 4 instead of ring position 2. The structures of 1a, 1b, 2a and 3b were confirmed by elemental analysis, ES-MS, FAB-MS, 1H and 13C NMR and IR spectroscopy.

Kristallstruktur von Acetonitril-trichlorocobaltat(II) Synthese und Struktur von 2,6-Dimorpholino-4-phenyl-1,3,5-oxadiazinium-Salzen / Crystal Structure of Acetonitrile Trichlorocobaltates(II) Synthesis and Structure of 2,6-Dimorpholino-4-phenyl-1,3,5-oxadiazinium Salts

Reactions of tris[(N-morpholinothiocarbonyl)benzamidato]cobalt(III) and of the free ligand in the presence of CoCl2, with SOCl2 in acetonitrile yield stable acetonitrile trichlorocobaltate(II) salts with 2,6-dimorpholino-4-phenyl-1,3,5-oxadiazinium cations, suitable for X-ray structure determination. Space group P21,/n, Z = 4, 4387 observed unique reflexions, R = 0.049, Lattice dimensions (22 °C): a = 772.94(9), b = 1611.5(4), c = 1911.1(5) pm; β = 96.23(2)°.