Showing papers by "Bernt Krebs published in 1984"

Synthetic route to [Fe6S9(SR)2]4- clusters (R = alkyl). Their spectroscopic and magnetic properties and the solid-state structures of [Fe6S9(SCH2Ph)2]4- and [(Fe6S9(SMe)2)2Na2]6-

Abstract: Determination par diffraction RX des structures des complexes (Et 4 N) 4 [Fe 6 S 9 (SCH 2 Ph) 2 ].H 2 O et (Et 4 N) 6 [(Fe 6 S 9 (SMe) 2 ) 2 Na 2 ]. Mesure de la susceptibilite magnetique du premier complexe et etude par spectre IR, RMN et electronique des deux complexes et du complexe (Et 4 N) 4 [Fe 6 S 9 (SEt) 2 ]

[Cu12S8]4⊖: ein geschlossener binärer Kupfer(i)‐sulfid‐Käfig mit kubooktaedrischer Metall‐ und kubischer Schwefelanordnung

Abstract: Etude RX du sel [Ph 4 P] 4 [Cu 12 S 8 ]: cristallisation dans P2 1 /n avec Z=2; affinement jusqu'a R=0,037

NMR studies of the system BSTl

Abstract: 11B, 203Tl and 205Tl NMR studies of glasses in the system Tl2SB2S3 have shown striking similarities to borate glasses. For low thallium contents, the fraction N4 of four-coordinated boron atoms increases in proportion to R = mol.% Tl2S/mol.% B2S3, and the monovalent thallium is tetrahedrally coordinated by sulfur. N4 reaches a maximum near R = 0.5, and discontinuous changes of the thallium bonding state towards more covalency is indicated at high Tl contents. Detailed information about the structural units and the precipitation of crystalline phases is obtained from the NMR and X-ray data. Differences between oxide and non-oxide systems are discussed.

NbAlCl8: a molecular dinuclear complex in the solid, melt, and vapor phases. Synthesis, crystal structure, and Raman spectra

Abstract: Cristallisation dans Cmcm avec a=8,016, b=17,139 et c=8,116 A, Z=4; affinement jusqu'a R=0,030. Les cristaux contiennent des molecules dinucleaires Cl 4 NbCl 2 AlCl 2 avec la symetrie mm, consistant en un tetraedre AlCl 4 partageant une arete avec un octaedre NbCl 6 deforme. Spectres Raman polarises de monocristaux a temperature ambiante et de melanges fondus NbCl 5 , AlCl 3 , ainsi que de vapeurs mixtes. Attribution des bandes de ces differents spectres

Preparation and crystal structure of a sulphinylnitrilo complex of rhodium(I): trans-[Rh(CO)(NSO)(PPh3)2]

Abstract: The reaction of CsNSO2 with [RhH(CO)(PPh3)3] in acetonitrile yields trans-[Rh(CO)(NSO)(PPh3)2](1) and PPh3O. Complex (1) has been characterised by elemental analyses, i.r. spectra, and a single-crystal X-ray structure investigation. Crystals of (1) are triclinic, space group P, with a= 9.248(2), b= 9.502(2), c= 10.567(2)A, α= 71.52(2), β= 89.71 (2), γ= 69.80(2)°, and Z= 1. In the square-planar molecular complex the carbonyl group [Rh–C 1.843(6)A] is in the trans position relative to the NSO ligand [Rh–N 1.989(9), N–S 1.48(1), S–O 1.51(1)A; N–S–O 122.5(5)°]. The Rh–P bond lengths to the trans-Co-ordinated phosphine ligands are 2.330(1)A. The arrangement of the molecules in the crystal is disordered, with a superposition of two half-occupied CO and NSO ligand sites in the electron-density map, simulating the crystallographic inversion centre at the Rh site.

Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10]

Abstract: On heating of [(C₂H₅)₄N][OsCl₆] for a short time at 240 °C , Cl₂ is lost and [(C₂H₅)₄N]₂[Os₂Cl₁₀] is formed quantitatively Both complexes are connected by a temperature dependent redox equilibrium so that by treatment at 120 °C with Cl₂ gas the hexachloroosmate(V) is recovered from the decachlorodiosmate(IV) The crystal structures of salts of both an ions were determined from single crystal X -ray diffraction analyses [(C₂H₅)₄N][OsCl₆] is monoclinic, space group P2 ₁ with a = 7 020 (1), b = 10 163 (2), c = 11609 (2) A , β = 10391(1)° (at - 133 °C) The strongly pseudocentrosymmetric structure shows a reversible phase transition at ca 85 °C The Os -Cl bond length (mean value 2303 A) in the regular [OsCl₆]-octahedra is significantly smaller than in [OsCl₆]²⁻ , in accordance with vibrational spectra [(n -C₄H₉)₄N]₂ [Os₂Cl₁₀] crystallizes in the orthorhombic space group Pbca with a = 15 496 (2), b = 15 965 (3), c = 19 431(3) A and contains centrosymmetric [Os₂Cl₁₀]²⁻ ions with approximate D₂ₕ symmetry Within the edge-sharing [OsCl₆] octahedra the mean terminal and bridging Os -Cl bond lengths are 2307 and 2411 A , respectively

Vanadium‐Thilat‐Komplexe mit VS5‐und VOS4‐Zentren: Synthese und Struktur von [VS(SC2H4S)2]2⊖ und Na2[VO(SC2H4S)2].8 MeOH

Abstract: Preparation par reduction de VS 4 3− avec l'ethanedithiolate-1,2 et isole sous forme de sel de tetraphenylphosphonium

Synthesis and structure of [Ph4P]2[Cu6(S4)3S5], a polycyclic hexanuclear copper(I) cluster with complete sulphur co-ordination

Abstract: The reaction of a methanolic CuI–thiolate solution with elemental sulphur yields deep-red[CU6(S4)3S5]2–which is the first hexanuclear CuIcluster with the complete sulphur co-ordination; the polycyclic anion can be regarded as an inorganic analogue of a corresponding mixed thiolate-sulphide complex and thus can serve as a possible model for cuI–thiolate sites in biological systems.

Ein neuer Wasserstoffbrücken-Typ: intramolekulare S-H...S-Brücken in Dithiotropolon

Abstract: Mise en evidence de ce nouveau type de liaison a partir d'etude spectrometrique et par determination de la structure cristalline du compose du titre (groupe P2 1 /c avec a=8,352, b=13,806 et c=12,371 A, β=103,46°, Z=8

Synthetic route to (fe6s9(sr)2)4- clusters (r = alkyl). their spectroscopic and magnetic properties and the solid-state structures of (fe6s9(sch2ph)2)4- and ((fe6s9(sme)2)2na2)6-

Abstract: Determination par diffraction RX des structures des complexes (Et 4 N) 4 [Fe 6 S 9 (SCH 2 Ph) 2 ].H 2 O et (Et 4 N) 6 [(Fe 6 S 9 (SMe) 2 ) 2 Na 2 ]. Mesure de la susceptibilite magnetique du premier complexe et etude par spectre IR, RMN et electronique des deux complexes et du complexe (Et 4 N) 4 [Fe 6 S 9 (SEt) 2 ]

Bromoselenate(II): Darstellung, Struktur und Eigenschaften von [P(C6H5)4]2SeBr4 und [P(C6H5)4]2Se2Br6

Abstract: Les deux composes cristallisent dans le systeme triclinique, groupe P1. Le premier compose est forme d'anions monomeres SeBr 4 2− avec une coordination plan carre autour de Se(II). Le meme type de coordination est observe dans les anions centrosymetriques Se 2 Br 6 2−