Darstellung,Mössbauer- und Schwingungsspektren der Komplexe [SnCl4F]⊖, [SnCl4(NCS)]⊖ und [SnCl4(NCS)2]2⊖

Preparation, Mössbauer and Vibrational Spectra of the Complexes [SnCl₄F]^?, [SnCl₄(NCS)]^?, and [SnCl₄(NCS)₂]^2? N(CH₂)₄F and N(CH₂)₄SCN react in liquid SO₂ with SnCl₄ yielding the adducts [N(CH₃)₄][SnCl₄F] (I), [N(CH₃)₄][SnCl₄(NCS)] (II) and [N(CH₃)₄]₂[SnCl₄(NCS)₂] (III).respectively. Mössbauer and vibrational spectra indicate for the anion of I a fluoro-bridged species, which is probably tetrameric like the isoelectronic SbCl₄F. For II dimeric moieties are proposed with bridging S-atoms, while [SnCl₄(NCS)₂]^2? has an octahedral structure with N-bonded isothiocyanate groups in the trans-positions.     

Synthese und Schwingungsspektrum des [Ta2OCl10]2⊖-Ions

Synthesis and Vibrational Spectrum of the [Ta₂OCl₁₀]^2? Ion (PPh₄)₂[Ta₂OCl₁₀] is prepared from NO[TaOCl₄] with tetraphenylphosphonium chloride. The vibrational spectrum is in accordance with the D_4h symmetry of the m?-Oxo-decachloroditantalum(V) ion.     

Die Bromokomplexe von Molybdän(IV) [MoBr6]2⊖ und [Mo2Br10]2⊖. Die Kristallstruktur von (PPh3Me)2[MoBr6] · 2 CH2Br2

Bromo Complexes of Molybdenum(IV) [MoBr₆]^2? and [Mo₂Br₁₀]^2?. Crystal Structure of (PPh₃Me)₂[MoBr₆] · 2 CH₂Br₂ The bromomolybdates(IV) (PPh₃Me)₂[MoBr₆] · 2 CH₂Br₂ and (PPh₄)₂[Mo₂Br₁₀] are obtained by reactions of molybdenum tetrabromide with PPh₃MeBr and PPh₄Br, respectively. They form black-brown, hydrolysis sensitive crystal powders. The crystal structure of (PPh₃Me)₂[MoBr₆] · 2 CH₂Br₂ was determined by X-ray diffraction (2376 independent observed reflexions, R = 0.082). Crystal data: a = 1024, b = 1131, c = 1179 pm, α = 108.2°, β = 106.8°, γ = 99.0°, space group P1 , Z = 1. The compound consists of PPh₃Me⁺ ions, CH₂Br₂ molecules and nearly octahedral [MoBr₆]^2? ions with MoBr bond lengths between 252.7 and 254.0 pm.