Sulfonazo (I) und sein Dibrom (II)- und Dimethylderivat (III)

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Lumineszierende Cu(I)- und Ag(I)-Cluster mit Thionoliganden

Zusammenfassung Cu(I) bildet mit zahlreichen nicht lumineszierenden Thionoliganden (N-monosubstituierten N-Sulfonylthioharnstoffen, N,N-Dialkyl-N-phenylthioharnstoffen und N,N-Dialkylmonothiocarbamaten) rot lumineszierende oktaedrische Cluster (CuL)₆. Die Lumineszenz tritt sowohl im Festzustand als auch in Lösungen auf. Abklingzeiten von 10^–5s deuten auf kurzlebige Phosphoreszenz hin. Der Einfluß verschiedener Strukturelemente auf die Lage der Emissionsmaxima wird diskutiert. Dabei bewirken Veränderungen in der Metall-Ligand-Koordination die stärkste Verschiebung der Lumineszenzbanden. Tetraedrische (CuL)₄-Cluster mit den obigen Thionoliganden zeigen keine Lumineszenz. Generelle Unterschiede in der Struktur oktaedrischer und tetraedrischer Cluster werden diskutiert.Ag(I) bildet nur mit N-Alkyl-N-sulfonylthioharnstoffen lumineszierende Cluster (AgL)₆. Die Lumineszenz ist im Gegensatz zu den Cu-Clustern auf den Festzustand beschränkt.

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Luminescent Cu(I) and Ag(I) clusters with thiono ligands

Summary Octahedrical (CuL)₆ clusters with several non luminescent thiono ligands (N-monosubstituted N-sulfonylthioureas, N,N-dialkyl-N-phenylthioureas and N,N-dialkylmonothiocarbamates) show red luminescence in the solid state and in solution. The luminescence lifetimes of 10^–5s are typical of short lived phosphorescence. The emission bands are affected by structural variation of the ligand. Changes of the coordination bonds cause the strongest shifts of the luminescence maxima. Tetrahedrical (CuL)₄ clusters with the same thiono ligands are not luminescent. General structural differences between octahedral and tetrahedral clusters are discussed.(AgL)₆ clusters are only luminescent in the solid state and if the ligand is a N-monosubstituted N-sulfonylthiourea

     

Alkylidentriphenylphosphoran-komplexe von kupper(I)- und silber(I)-chlorid: I. 21 komplexe

Ylide complexes of the type [(C₆H₅)₃PCHRMCHRP(C₆H₅)₃]Cl (M = Cu, Ag) have been obtained from the reaction of methylene, ethylidene- and isobutylidene-triphenylphosphorane with CuCl and AgCl. These organocopper and organosilver compounds are of surprisingly high thermal stability. In the ¹H, ¹³C and ³¹P NMR spectra of the silver compound (R = H) the spin—spin interactions ¹HC^107,109 Ag, ³¹PC^107,109 Ag, and for the first time, ¹³C^107,109 Ag could be detected.     

Die Reaktionen von Diphenylcarboazid (DI) und Diphenylcarbazon (DO) mit Quecksilber(I)- und Quecksillber(II)-ionen

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Die Oxydation von Vanadium(II), -(III) und -(IV) durch Jod(I)-chlorid

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Darstellung und Kristallstrukturen von Dicyanamido(triphenylphosphan)gold(I) und Nitrosodicyanmethanido(triphenylphosphan)gold(I)

Preparation and Crystal Structures of Dicyanamido(triphenylphosphane)gold(I) and Nitrosodicyanomethanido(triphenylphosphane)gold(I) The coordination compounds [(Ph₃P)Au{N(CN)₂}] ( 1 ) and [(Ph₃P)Au{ONC(CN)₂}] ( 2 ) are obtained by the reaction of [Au(PPh₃)]NO₃ with Na[N(CN)₂] or K[ONC(CN)₂] in CH₂Cl₂. The compounds are characterized by IR spectroscopy and by crystal structure determination. 1 crystallizes triclinic in the space group P 1 with a = 930.16(4), b = 1011.89(13), c = 1118.35(16) pm, α = 115.327(10), β = 90.899(8), γ = 103.394(8)°, Z = 2. 2 crystallizes monoclinic in the space group P2₁/n with a = 832.59(10), b = 1139.30(16), c = 2078.9(4) pm, β = 99.84(2)°, Z = 4. The crystal structures of both compounds are built up by pairs of antiparallel oriented molecules with linear coordinated gold atoms and weak intermolecular Au–N‐interactions.     

Zwei- und dreikernige Komplexe des WS42– mit Tricarbonylrhenium(I)- und -mangan(I)-Fragmenten: Struktur,Spektroskopie und Elektrochemie

Di- and Trinuclear Complexes of WS₄^2– with Tricarbonylrhenium(I) and -manganese(I) Fragments: Structure, Spectroscopy, and Electrochemistry The reaction of (NEt₄)₂WS₄ with two equivalents of M(CO)₅(O₃SCF₃), M = Mn or Re, in acetonitrile yielded the crystallographically characterized neutral compounds [(CH₃CN)(OC)₃M(μ-S₂WS₂)M(CO)₃(NCCH₃)]. The individual molecules are chiral and contain WS₄ and MS₂(CO)₃(CH₃CN) moieties in approximately tetrahedral and octahedral configurations, respectively. Vibrational and electronic absorption spectra are in agreement with the crystal structure, comparable results were obtained for trinuclear complexes [(L)(OC)₃Re(μ-S₂WS₂)Re(CO)₃(L)](NEt₄)₂, L = Cl^– or CN^–, and for the dinuclear systems [(WS₄)Re(CO)₃(CH₃CN)](NEt₄) and [(WS₄)Re(CO)₃Cl](NEt₄)₂. Electrochemical processes are irreversible due to the lability of acetonitrile or chloride ligands in corresponding complexes, however, the cyanide compound [(NC)(OC)₃Re(μ-S₂WS₂)Re(CO)₃(CN)]^2– showed reversible one-electron reduction to a first tetrathiotungstate(V) species as detected by UV/Vis/IR spectroelectrochemistry.     

Die arsenometrische Bestimmung von Kupfer(I)- und Kupfer(II)-ionen nebeneinander

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Blei und Thallium(I)

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Oleandomycin (I) und Tetracyclin (II)

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Alkylidentriphenylphosphoran-komplexe von kupfer(I)- und silber(I)-chlorid : II. 1/1-komplexe

Stable 1/1 complexes have been obtained from the ylides methylene, ethylidene and isobutylidene triphenylphosphorane with CuCl, and from (C₆H₅)₃-P=CH₂ and AgCl. In these organometallic compounds of copper and silver the ylides are attached to the metal through the carbanionic donor atom. A cubane-type structure is proposed for the oligomers of the general formula [(C₆H₅)₃-PCHR·MCl]_n, (M = Cu, Ag; R = H, CH₃, CH(CH₃)     

Darstellung und Charakterisierung von Chrom(V)- und Mangan(V)- nitridophthalocyaninen(1-) und -(2-): [MNPc(1-)]+; und [MNPc(2-)] (M=Cr,Mn)

Preparation and Characterization of Chromium of Chromium(V)- and Manganese(V)- nitridophthalocyanines(1-) and -(2-): [MNPc(1-)]⁺ and [MNPc(2-)] (M=Cr, Mn) Nitridophthalocyaninatochromium(V), [CrNPc(2-)], is prepared by oxidation of [Cr(OH)₂PC(2-)] with chlorine in the presence of excess ammonia as a paramagnetic (μ_eff = 1,99 B.M.), Microcrystalline blue powder. Through chemically very stable it reacts as well as the isostructural nitridophthalocyaninatomanganese(V) with bromine or concentrated nitric acid giving ring- oxidized darkblue nitridophthalocyaninatomental(poly)bromides or -nitrates, [MNPc(1-)]X (M=Cr, Mn; X=Br_y, NO₃; y≈?2). The nitrido-metal stretching vibration (ν(N?M)) is independent of the oxidation state of the Pc-ligands at ca. 1017 cm^?1 for the chromium and at ca. 1055 cm^?1 for the manganesenitridophthalocyanines. ν(N?Mn) is resonance Raman (r.r.) enhanced, ν(N?Cr) not. The characteristic differences in the u.v. -vis., f.i.r./m.i.r. and r.r. spectra of [MNPc(2-)] and [MNPc(1-)⁺ and the influence of aggregation of phthalocyanine-radicals are discussed.     

Glucosamin(I) und Galaktosamin(II)

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