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  • Inorganic Chemistry  (1,340)
  • 1995-1999  (567)
  • 1990-1994  (773)
  • 1950-1954
  • 1995  (567)
  • 1991  (773)
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  • 1995-1999  (567)
  • 1990-1994  (773)
  • 1950-1954
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  • 101
    Electronic Resource
    Electronic Resource
    Bi5,6Ni5I: Eine partiell oxidierte intermetallische Phase mit Kanalstruktur (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2034-2042 
    Details
    ISSN: 0044-2313
    Keywords: Bismuth nickel iodide ; subhalide ; crystal structure ; chemical bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bi5,6Ni5I: A Partly Oxidized Intermetallic Phase with Channel StructureBi5,6Ni5I was prepared from the elements by chemical vapour deposition. Single-crystal investigations (space group I2/m, a = 1 852.1(3), b = 418.45(6), c = 1 373.8(3) pm, β = 90.42(2)°, V = 1 064.7(3) · 106 pm3) revealed parallel doublewalled channels of nickel and bismuth atoms. The central pseudo 5 axis of each channel is occupied by 6/5 disordered bismuth atoms per lattice translation along [010]. Double rows of iodine atoms fill the distorted hexagonal arrangement of the channels. Bi5,6Ni5I is stabilized by metallic bonding in the framework metal atoms and additional heteropolar interactions between bismuth and iodine atoms as well as between bismuth and nickel atoms. Bi5,6Ni5I shows metallic conductivity and ferromagnetic ordering below 17 K.
    Notes: Bi5,6Ni5I wurde aus den Elementen durch eine chemische Transportreaktion dargestellt. In der an einem Einkristall bestimmten Struktur (Raumgruppe I2/m, a = 1 852,1(3), b = 418,45(6), c = 1 373,8(3) pm, β = 90,42(2)°, V = 1 064,7(3) · 106 pm3) liegen parallele, doppelwandige Röhren aus Nickel- und Bismutatomen vor. Auf der zentralen Pseudo-5-Achse jedes Kanals finden sich fehlgeordnet 6/5 Bismutatome pro Translationseinheit in Richtung [010]. Die Iodatome bilden Doppelreihen in der verzerrt hexagonalen Anordnung der Röhren. Die Stabilität von Bi5,6Ni5I resultiert aus der metallischen Bindung im Metallatomgerüst sowie aus heteropolaren Wechselwirkungen sowohl zwischen Bismut- und Iodatomen als auch zwischen Bismut- und Nickelatomen. Bi5,6Ni5I ist metallisch leitend und ordnet unterhalb 17 K ferromagnetisch.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956211210
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  • 102
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    Neue ein- und mehrkernige Komplexe der Lanthanoiden. Zur Reaktion von Ph2Se2 mit Ytterbium (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2043-2048 
    Details
    ISSN: 0044-2313
    Keywords: Ytterbium compounds ; complexes with selenolatoligands ; crystal structure ; mixed valent compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Mono- and Polynuclear Complexes of the Lanthanides. On the Reaction of Ph2Se2 with YtterbiumSurprising formation of different complexes during the reaction of Ytterbium with Dichalcogenides. With THF is the mononuclear complex [Yb(SePh)3(thf)3] 1 (space group P31c (No. 159), Z = 2, a = 15.353(3) Å, c = 7.8920(10) Å) built up. In this compound is the Lanthanidion octahedrally souronded by the ligands. Reaction in Toluol/THF leads in contrast to the tetranuclear complex [Yb4(SePh)8O2(thf)6] 2 (space group C2/c (No. 14), Z = 4, a = 27.084(9) Å, b = 13.021(4) Å, c = 24.002(8) Å, β = 106.13(3)°). In DME it is possible to isolate the ionic species [Yb3(SePh)6(dme)4][Yb(SePh)4(dme)] 3 (space group P1 (No. 2), Z = 2, a = 11.109(3) Å, b = 11.664(2) Å, c = 36.303(10) Å, α = 84.60(4)°, β = 89.52(3)°, γ = 73.69(2)°). In this reactions are neutral and also ionic complexes accesible.
    Notes: überraschende Produktvielfalt bei der Reaktion von Ytterbium mit Dichalkogeniden. In THF bildet sich der einkernige Komplex [Yb(SePh)3(thf)3] 1 (Raumgruppe P31c (Nr. 159), Z = 2, a = 15,353(3) Å, c = 7,8920(10) Å). In dieser Verbindung ist das Zentralion oktaedrisch von den Liganden umgeben. Reaktion in Toluol/THF führt dagegen zu der vierkernigen Ytterbiumverbindung [Yb4(SePh)8O2(thf)6] 2 (Raumgruppe C2/c (Nr. 14), Z = 4, a = 27,084(9) Å, b = 13,021(4) Å, c = 24,002(8) Å, β = 106,13(3)°). In DME erhält man die ionische Komplexverbindung [Yb3(SePh)6(dme)4][Yb(SePh)4(dme)] 3 (Raumgruppe P1 (Nr. 2), Z = 2, a = 11,109(3) Å, b = 11,664(2) Å, c = 36,303(10) Å, α = 84,60(4)°, β = 89,52(3)°, γ = 73,69(2)°). Durch diese Reaktionen sind neutrale und ionisch aufgebaute Ytterbiumkomplexe zugänglich.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956211211
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  • 103
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    Synthese und Kristallstrukturen von (Ph4P)4[Bi8I28], (nBu4N)[Bi2I7] und (Et3PhN)2[Bi3I11] - Iodobismutate mit isolierten bzw. polymeren Anionen (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2049-2054 
    Details
    ISSN: 0044-2313
    Keywords: Iodobismuthate ; [Bi2I7]-, [Bi3I11]2-, [Bi8I28]4-, crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of (Ph4P)4[Bi8I28], (nBu4N)[Bi2I7], and (Et3PhN)2[Bi3I11] - Bismuth Iodo Complexes with Isolated and Polymeric AnionsSolutions of BiI3 in methanol react with NaI and (nBu4N)(PF6) or (Et3NPh)(PF6) to form anionic bismuth iodo complexes (nBu4N)[Bi2I7] 1 and (Et3PhN)2[Bi3I11] 2. In 1 Bi4I16 units, and in 2 Bi6I24 units are linked by common I-atoms to onedimensional infinite chains. Reaction of BiI3 with (Ph4P)(PF6) in methanol yields (Ph4P)4[Bi8I28] 3. The anions of 1-3 consist of edge-sharing BiI6 octahedra.(nBu4N)[Bi2I7] 1: Space group I2/m (No. 13), a = 1 082.3(5), b = 2 597.1(13), c = 1 206.1(6) pm, β = 93.17(2)°, V = 3 385(3) · 106 pm3;(Et3PhN)2[Bi3I11] 2: Space group P1 (No. 2), a = 1 283.5(6), b = 1 345.9(7), c = 1 546.3(8) pm, α = 83.87(2), β = 74.24(2), γ = 68.26(2)°, V = 2 388(2) · 106 pm3;(Ph4P)4[Bi8I28] 3: Space group P1 (No. 2), a = 1 329.3(4), b = 1 337.0(4), c = 2 193.1(5) pm, α = 104.20(2), β = 99.73(2), γ = 100.44(2)°, V = 3 622(2) · 106 pm3.
    Notes: BiI3 reagiert in methanolischer Lösung mit NaI und (nBu4N)(PF6) bzw. (Et3PhN)(PF6) zu (nBu4N)[Bi2I7] 1 und (Et3PhN)2[Bi3I11] 2 mit Iodobismutatanionen. In 1 liegen unendliche Stränge von über gemeinsame I-Atome verknüpften Bi4I16-Einheiten vor. In 2 bilden verkettete Bi6I24-Einheiten polymere Anionen. Führt man die Umsetzung von BiI3 mit (Ph4P)(PF6) ohne NaI durch, so kristallisiert aus Methanol (Ph4P)4[Bi8I28] 3. Die Anionen von 1-3 bestehen aus kantenverknüpften BiI6-Oktaedern.(nBu4N)[Bi2I7] 1: Raumgruppe I2/m (Nr. 13), a = 1 082,3(5), b = 2 597,1(13), c = 1 206,1(6) pm, β = 93,17(2)°, V = 3 385(3) · 106 pm3;(Et3PhN)2[Bi3I11] 2: Raumgruppe P1 (Nr. 2), a = 1 283,5(6), b = 1 345,9(7), c = 1 546,3(8) pm, α = 83,87(2), b = 74,24(2), γ = 68,26(2)°, V = 2 388(2) · 106 pm3;(Ph4P)4[Bi8I28] 3: Raumgruppe P1 (Nr. 2), a = 1 329,3(4), b = 1 337,0(4), c = 2 193,1(5) pm, α = 104,20(2), β = 99,73(2), γ = 100,44(2)°, V = 3 622(2) · 106 pm3.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956211212
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  • 104
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    über die Reaktionen von CH3OCl, CF3OCl, CF3OF und CF3OH mit dem supersauren System HF/MF5 (M = As, Sb) Darstellung und Charakterisierung von CH3OCl(H)+MF6- und CF3OCl(H)+MF6- (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2055-2060 
    Details
    ISSN: 0044-2313
    Keywords: Chlorine trifluoromethyloxonium-, chlorine methyloxonium hexafluoroantimonate and -arsenate ; vibrational, nmr, mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reactions of CH3OCl, CF3OCl, CF3OF, and CF3OH with the Superacid System HF/MF5 (M = As, Sb). Preparation and Characterization of CH3OCl(H)+MF6- and CF3OCl(H)+MF6-The preparation of the chlorine oxoniumsalts CH3OCl(H)+MF6- and CF3OCl(H)+MF6- by protonation of CH3OCl and CF3OCl in the superacid solution of HF/MF5 (M = As, Sb) is described. However CF3OF and CF3OH have not been protonated under the same conditions. In the case of CF3OH the formation of F2CO · MF5 is observed. The novel compounds are characterized by nmr- and vibrational spectroscopy.
    Notes: Es wird über die Darstellung der Chloroxoniumsalze CH3OCl(H)+MF6- und CF3OCl(H)+MF6- durch Protonierung von CH3OCl und CF3OCl in dem supersauren System HF/MF5 (M = As, Sb) berichtet. Dagegen lassen sich CF3OF und CF3OH bei gleichen Bedingungen nicht protonieren. CF3OH bildet in supersaurer Lösung die Addukte F2CO · MF5. Die Charakterisierung aller neuen Verbindungen erfolgt NMR- und schwingungsspektroskopisch.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956211213
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  • 105
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    Synthese, Kristallstruktur und spektroskopische Charakterisierung von Tetraphosphorhexaoxid-monoselenid, P4O6Se (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2065-2069 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphosphorus hexaoxide monoselenide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure, and Spectroscopic Characterization of Tetraphosphorus Hexaoxide Monoselenide, P4O6SeP4O6Se has been synthesized by photochemical reaction between P4O6 and elemental selenium in CS2 in presence of iodine as a catalyst. Single crystals form at purification via sublimation. The compound (m. p. 46°C) crystallizes in the monoclinic space group P21/c (no. 14) with a = 1 051.8(2), b = 652.9(1), c = 1 178.6(2) pm, β = 109.29(1)°, Z = 4. Within the limits of experimental error, the molecules exhibit C3v symmetry. IR, Raman, and 31P n.m.r. (solution) spectra of the compound are reported and discussed. The geometry of the Molecule as determined by theoretical methods (SCF level) is in good agreement with the experimental results.
    Notes: P4O6Se wurde durch photochemische Reaktion von P4O6 mit elementarem Selen in CS2 in Gegenwart von Iod als Katalysator dargestellt; Einkristalle entstanden bei der Reinigung durch Sublimation. Die Verbindung (Fp. 46°C) kristallisiert in der monoklinen Raumgruppe P21/c (Nr. 14) mit a = 1 051,8(2), b = 652,9(1), c = 1 178,6(2) pm, β = 109,29(1)°, Z = 4. Im Rahmen der Fehlergrenzen der Strukturbestimmung besitzen die Moleküle C3v-Symmetrie. IR-, Raman- und 31P-Lösungs-NMR-Spektren der Verbindung werden mitgeteilt und diskutiert. Die mit quantenchemischen Methoden auf SCF-Niveau berechnete Molekülgeometrie stimmt mit der experimentell bestimmten gut überein.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956211215
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  • 106
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    Synthese, Struktur und magnetische Eigenschaften von [CrCl(μ-Cl)(TMEDA)]2 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2061-2064 
    Details
    ISSN: 0044-2313
    Keywords: Chromium(II) chloride TMEDA complex ; crystal structure ; magnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and Magnetic Properties of [CrCl(-μCl)(TMEDA)]2The title complex [CrCl(μ-Cl)(TMEDA)]2 (1) is obtained in an equimolar reaction of CrCl2(THF) with TMEDA in high yield. 1 crystallises in the monoclinic space group P21/c with a = 843.2(2), b = 1 109.(2), c = 1 147.4(3) pm, β = 102.99(2)° and Z = 2. The molecular structure of 1 contains two, slightly distorted quadratic pyramidal CrL5-subunits, which are linked via two unsymmetrical Cl-bridges. The μ-Cl-functions take the apical position of one and a basal position of the second CrL5-unit, wherein the apical Cr-Cl bond (277.6(1) pm) is destinctly longer than the basal Cr-Cl bond (240.6(1) pm). The terminal Cr-Cl bond is still shorter (237.5(1) pm). The Cr…Cr distance is far beyond any bonding interaction. This is confirmed by means of magnetic susceptibility measurements, which show four unpaired electrons per Cr centre; however, a small antiferromagnetic coupling of J/k = -7.3 K can be calculated. This coupling is suggested to be originated by a 90°-σ-superexchange via the asymmetric μ-Cl functions.
    Notes: Den Titelkomplex [CrCl(μ-Cl)TMEDA]2 (1) erhält man in einer äquimolaren Reaktion von CrCl2(THF) mit TMEDA in hohen Ausbeuten. 1 kristallisiert in der monoklinen Raumgruppe P21/c mit a = 843,2(2), b = 1 109,4(2), c = 1 147,4(3) pm, β = 102.99(2)° und Z = 2. Die Molekülstruktur von 1 enthält zwei leicht verzerrte quadratisch pyramidal koordinierte CrL5-Untereinheiten, die über zwei unsymmetrische Cl-Brücken verbunden sind. Die μ-Cl-Funktionen nehmen die apikale Position der einen und eine basale Position der anderen CrL5-Einheit ein, wobei die apikale Cr-Cl-Bindung (277,6(1) pm) deutlich länger als die basale Cr-Cl-Bindung (240,6(1) pm) ist. Die terminale Cr-Cl-Bindung ist noch kürzer (237,5(1) pm), Der Cr—Cr-Abstand mit 381,7(1) pm liegt deutlich außerhalb einer bindenden Cr-Cr-Wechselwirkung. Dieses wird durch magnetische Suszeptibilitätsmessungen bestätigt, die pro Cr-Zentrum vier ungepaarte Elektronen nachweisen; allerdings kann eine kleine antiferromagnetische Kopplung von J/k = -7,3 K berechnet werden. Diese Kopplung wird vermutlich durch einen 90°-σ-Superaustausch über die Cl-Brücken erwirkt.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956211214
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  • 107
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    Preparation, crystal structure, and infrared characterization of the first thiocyanato-oxy-antimonate(III) [(CH3)4N]2[Sb6O4(NCS)12] (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2070-2074 
    Details
    ISSN: 0044-2313
    Keywords: Antimony(III) thiocyanate complex ; crystal structure ; IR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung, Kristallstruktur und IR-Charakterisierung des ersten Thiocyanato-oxyantimonats(III), [(CH3)4N]2[Sb6O4(NCS)12][(CH3)4N]2[Sb6O4(NCS)12] ist der erste Thiocyanato-oxyantimonat(III)-Komplex. Die Synthese, wichtige IR-Daten und die Struktur werden mitgeteilt. Die Verbindung kristallisiert in der triklinen Raumgruppe P1, Z = 2 (C10H12N7O2S6Sb3), a = 11,314(6), b = 12,846(3), c = 8,679(2) Å, α = 91,93(3)°, β = 90,31(3)°, γ = 99,13(3)°. Die Struktur wird aus zentrosymmetrischen [Sb6O4(NCS)12]2--Anionen und isolierten Tetramethylammonium-Kationen aufgebaut. Das grundlegende Strukturelement des Anions wird von drei SbOSbO-Ringen gebildet, die zu einem in zick-zack-Form, leicht gefalteten Band verbunden sind. Etwas Besonderes ist die Ungleichheit der sechs Thiocyanat-Liganden, obwohl alle N-gebunden an Antimon sind. Drei Thiocyanate sind terminal, während drei andere asymmetrisch N-verbrückend zwischen zwei Zentren sind; zwei von diesen verbinden die Anionen über Sb⋅⋅⋅S-Kontakte. Für die Antimonatome sind drei unterschiedliche Umgebungen vorhanden, einmal die Bindung an einen Stickstoff und drei Sauerstoffe, zweitens an einen Sauerstoff und drei Stickstoffe und drittens an je zwei Sauerstoffe und Stickstoffe.
    Notes: The salt [(CH3)4N]2[Sb6O4(NCS)12] is the first identified thiocyanato-oxy-antimonate(III) complex. Reported are details of the synthesis, relevant infrared data and its x-ray structure. The compound crystallizes in the triclinic space group P1 with Z = 2 (C10H12N7O2S6Sb3) and unit cell dimensions a = 11.314(6), b = 12.846(3), c = 8.679(2) Å; α = 91.93(3)°, β = 90.31(3)° and γ = 99.13(3)°. It contains centrosymmetric [Sb6O4(NCS)12]2- anions packed with isolated tetramethyl-ammonium cations. The fundamental structural element of the anion is provided by the fusion of three SbOSbO rings forming a zig-zag portion of a ribbon, only slightly pleated. Peculiar is the unequivalence of the six thiocyanate ligands, though all primarily N-bonded to antimony atoms. Three thiocyanates are terminal while other three are asymmetrically N-bridging between two centers; two of this latter type are also interconnecting the anions via Sb⋅⋅⋅S contacts. There are three different antimony environments, the primary bonding at Sb being to one nitrogen and three oxygens, to one oxygen and three nitrogens and to two atoms of each type.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211216
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  • 108
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    Ba2(CN2)(CN)2 und Sr2(CN2)(CN)2 - die ersten gemischten Cyanamid-cyanide (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2075-2082 
    Details
    ISSN: 0044-2313
    Keywords: Alkaline-earth cyanamide cyanides ; syntheses ; crystal structure ; anti-NiAs structure type ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ba2(CN2)(CN)2 and Sr2(CN2)(CN)2 - the First mixed Cyanamide CyanidesThe mixed cyanamide-cyanides M2(CN2)(CN)2 (M = Ba, Sr) were synthesized by the reaction of Ba2N and SrCO3, respectively, with HCN at 630°C. The crystal structure of Ba2(CN2)(CN)2 was determined from single-crystal X-ray investigations at room temperature and -100°C; the isostructural Sr2(CN2)(CN)2 was refined using powder methods (P63/mmc; Ba2(CN2)(CN)2: a = 1 066.52(5) pm, c=696.82(3) pm; Sr2(CN2)(CN)2: a = 1 035.91(1) pm, c = 664.23(1) pm; Z = 4). The crystal structure is a partially filled defect variant of the anti-NiAs structure type with a distorted hexagonal close packed arrangement of M2+-ions. All CN22- and one quarter of the CN- ions occupy 3/4 of the octahedrally coordinated interstices, the remaining cyanide anions are located at 3/8 of the tetrahedral sites. In the crystal structure the CN- are coordinated to the cations both end-on and side-on. All anions can be distinguished by vibrational spectroscopy.
    Notes: Die gemischten Cyanamid-cyanide M2(CN2(CN)2 (M = Ba, Sr) wurden durch Umsetzung von Ba2N bzw. SrCO3 mit HCN bei 630°C synthetisiert. Die Bestimmung der Kristallstruktur von Ba2(CN2)(CN)2 erfolgte anhand von Röntgen-Einkristalluntersuchungen bei Raumtemperatur bzw. -100°C, die Struktur des isotypen Sr2(CN2)(CN)2 wurde aus Pulverdaten verfeinert (P63/mmc, Ba2(CN2)(CN)2: a = 1 066,52(5) pm, c = 696,82(3) pm; Sr2(CN2)(CN)2: a = 1 035,91(1) pm, c = 664,23(1) pm; Z = 4). Die Kristallstruktur läßt sich als partiell aufgefüllte Defektvariante des anti-NiAs-Typs mit einer verzerrt hexagonal dichten Packung von M2+-Ionen auffassen. Sämtliche CN22-- und ein Viertel der CN--Ionen besetzen 3/4 der Oktaederlücken, die restlichen CN--Einheiten 3/8 der Tetraederlücken. Im Kristallverband sind die CN--Ionen sowohl end-on als auch side-on an die Kationen koordiniert. Die Anionen sind schwingungsspektroskopisch unterscheidbar.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211217
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  • 109
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    Zur Bildung von Vinylverbindungen des Lanthans und LutetiumsProfessor Herbert W. Roesky zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2089-2092 
    Details
    ISSN: 0044-2313
    Keywords: Organo rare earth complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Preparation of Vinyl Compounds of Lanthanum and LutetiumAt reaction of permethyllanthanocene chloride with vinyl lithium coupling of vinyl groups takes place with formation of the butadiene complex [Li(dme)3][Cp2*La(C4H6)] (1). The corresponding lutetium compound yields the expected vinyl complex Cp2*Lu(CH=CH2) · LiCl · dme (4) with low stability. Furthermore, the more stable alkenyl compounds Cp2*LaCPh=CMe2 · 2 thf (2) and Cp2*LuCPh=CMe2 · MgCl2 · dme (3) could be obtained. The new complexes were characterized by their 1H and 13C-n.m.r. spectra.
    Notes: Permethyllanthanocenchlorid reagiert mit Vinyllithium unter Vinylkopplung zu dem Butadienkomplex [Li(DME)3] [Cp2*La(C4H6)] (1). Ausgehend von der entsprechenden Lutetiumverbindung konnte dagegen das gesuchte Cp2*Lu(CH=CH2) · LiCl · DME (4) als wenig beständige Substanz erhalten werden. Als stabilere Alkenylverbindungen werden das Cp2*LaCPh=CMe2 · 2 THF (2) und Cp2*LuCPh=CMe2 · MgCl2 · DME (3) beschrieben. Die Charakterisierung der Komplexe erfolgte durch ihre 1H- und 13C-NMR-Spektren.
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    URL: http://dx.doi.org/10.1002/zaac.19956211219
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  • 110
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    Ternäre Thalliumplatin- und Thalliumpalladiumchalkogenide Tl2M4X6. Synthesen, Kristallstruktur und Bindungsverhältnisse (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2083-2088 
    Details
    ISSN: 0044-2313
    Keywords: Transition metal chalcogenides ; platinum ; palladium ; melting reaction ; crystal structure ; Extended-Hückel-calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Thallium Platinum and Thallium Palladium Chalcogenides Tl2M4X6. Syntheses, Crystal Structures, and Bonding RelationsThe compounds Tl2Pt4S6, Tl2Pt4Se6, Tl2Pt4Te6 and Tl2Pd4Se6 can be synthesized by a melting reaction from the elements or by the reaction of thallium carbonate, transition metal powder and chalcogen powder in the temperature range between 400°C and 950°C. X-Ray investigations on single crystals and powdered samples revealed a new structure type for the compounds, that can be understood as stacking variant of the already known atom arrangement of the alkaline metal platinum chalkogenides A2Pt4X6 (A ≙ alkaline metal, X ≙ S, Se). The short distances thallium-platinum and thallium-palladium, respectively, as well as the results of Extended-Hückel-calculations indicate covalent bonds between the main group and transition metal atoms.
    Notes: Die Verbindungen Tl2Pt4S6, Tl2Pt4Se6, Tl2Pt4Te6 und Tl2Pd4Se6 sind durch Schmelzreaktionen aus den jeweiligen Elementen oder durch die Umsetzung von Thalliumcarbonat, Übergangsmetall- und Chalkogenpulver im Temperaturbereich zwischen 400°C und 950°C darstellbar. Röntgenographische Untersuchungen an Einkristallen und an pulverförmigen Proben ergaben, daß die Verbindungen in einem neuen Strukturtyp kristallisieren, der als Stapelvariante schon bekannter Atomanordnungen der Alkalimetallplatinchalkogenide A2Pt4X6 (A ≙ Alkalimetall, X ≙ S, Se) aufgefaßt werden kann. Die geringen Atomabstände Thallium-Platin bzw. Thallium-Palladium deuten in übereinstimmung mit den Ergebnissen von Extended-Hückel-Rechnungen auf eine kovalente Bindung zwischen dem Hauptgruppen- und dem übergangsmetall hin.
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    Monomeres Trilithium-tris[tert-butyldimethylsilylamido]phenylsilan, PhSi[NLi(THF)SiMe2CMe3]3 -- Darstellung und KristallstrukturProfessor Herbert W. Roesky zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2093-2096 
    Details
    ISSN: 0044-2313
    Keywords: Monomeric trilithium-tris(silylamido)silane ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Monomeric Trilithium-tris[tert-butyldimethylsilylamido]phenylsilane, PhSi[NLi(thf)SiMe2CMe3]3 - Synthesis and Crystal StructureLithiated tert-butyldimethylsilylamine reacts with trifluorophenylsilane in a molar ratio 2:1 or 3:1 to give the bis- and tris(silylamino)silanes 1 [(Me3CSiMe2NH)2SiFPh] and 2 [(Me3CSiMe2NH)3SiPh]. The trilithium derivative 3 [Me3CSiMe2NLi(thf)]3SiPh is obtained in the reaction of 2 with n-BuLi in hexane/thf. 3 crystallizes as a monomer forming three planar four-membered (LiNSiN)-rings. The results of the crystal structure of 3 are discussed.
    Notes: Lithiiertes tert-Butyldimethylsilylamin reagiert mit Trifluorphenylsilan im molaren Verhältnis 2:1 bzw. 3:1 zu den Bis- und Tris(silylamino)silanen 1 [(Me3CSiMe2NH)2 · SiFPh] und 2 [(Me3CSiMe2NH)3SiPh]. In der Reaktion von 2 mit n-BuLi in Hexan/THF entsteht das Trilithiumderivat 3 [Me3CSiMe2NLi(THF)]3SiPh. 3 kristallisiert als Monomer und bildet im Kristall drei planare, viergliedrige (LiNSiN)-Ringe. Die Ergebnisse der Kristallstrukturanalyse von 3 werden mitgeteilt.
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    A charge-stabilized Jahn-Teller Distortion of the Mixed Valence System NaBa2Cu3O6 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1508-1512 
    Details
    ISSN: 0044-2313
    Keywords: Jahn-Teller distortion ; Copper oxides ; Nickel oxides ; Electronic structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Eine ladungsstabilisierte Jahn-Teller-Verzerrung des gemischt-valenten Oxids NaBa2Cu3O6Die Kristallstruktur von NaBa2M3O6 enthält ungewöhnliche hexagonale Prismen aus verknüpften quadratischen MO4-Gruppen. Die Einheit mit M = Cu ist verzerrt, jedoch unverzerrt mit M = Ni. Berechnungen der elektronischen Struktur ergeben eine Orbitalentartung, und mit der Elektronenzahl für Cu führt eine Verzerrung zur (elektronischen) Stabilisierung. Die von der Zusammensetzung vorgegebene Oxidationsstufe des Metalls bestimmt die Art der besetzten und unbesetzten Metall-d-Orbitale und damit die bevorzugte Verzerrung.Die Ergebnisse geben vertieften Einblick in die Natur gemischt-valenter Verbindungen und ermuntern zur Präparation von Na2BaM3O6.
    Notes: The crystal structure of NaBa2M3O6 contains an unusual hexagonal prism composed of linked MO4 squares. This unit is distorted in the M = Cu compound but undistorted in the M = Ni material. Electronic structure calculations show an orbital degeneracy and electronic stabilization on distortion of the hexagonal prism at the electron count appropriate for the Cu compound. The preferred distortion is determined by considering how the nature of both the occupied and unoccupied metal d orbitals are consistent with the metal oxidation states set by the stoichiometry. The results provide added insights into the nature of mixed valence compounds. The synthesis of Na2BaM3O6 is encouraged.
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    Sulfur Compounds. 183. A Derivative of Perthiocarbonic Acid H2CS4: X-ray structural analysis of bis(triphenylmethyl) perthiocarbonate (Ph3C)2CS4 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1513-1516 
    Details
    ISSN: 0044-2313
    Keywords: Perthiocarbonic acid diester ; X-ray structural analysis ; perthiocarbonate ; bis(triphenylmethyl) perthiocarbonic acid diester ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ein Derivat der Perthiokohlensäure H2CS4: Röntgenstrukturanalyse von Bis(triphenylmethyl)perthiocarbonat (Ph3C)2CS4Die Molekülstruktur von Ph3CSSC(S)SCPh3 · CS2 wurde durch eine Röntgenstrukturanalyse bestimmt. Die Substanz kristallisiert im triklinen Kristallsystem [a = 884,9(2) pm, b = 1 039,5(2) pm, c = 2 064,6(3) pm, α = 75,86(1)°, γ = 79,83(2)°, γ = 77,31(5)°, Z = 2, Raumgruppe P1]. Die CS3-Gruppe ist planar; die S—S-Bindung (201,4 pm) bildet mit der CS3-Ebene einen Winkel von 5,7°. Der CSSC-Torsionswinkel beträgt 96,3°. (Ph3C)2CS4 wurde durch Umsetzung von TosNSCl2 (Tos = p-MeC6H4SO2) mit Ph3CSH in CS2 in Gegenwart von Triethylamin erhalten. Der Reaktionsmechanismus wird diskutiert.
    Notes: The molecular structure of Ph3CSSC(S)SCPh3 · CS2 has been determined by X-ray structural analysis. The substance crystallizes in the triclinic crystal system [a = 884.9(2) pm, b = 1 039.5(2) pm, c = 2 064.6(3) pm, α = 75.86(1)°, β = 79.83(2)°, γ = 77.31(5)°, Z = 2, space group P1]. The CS3 group is planar; the S—S-bond (201.4 pm) forms an angle of 5.7° with the CS3 plane. The torsional angle CSSC equals 96.3°. (Ph3C)2CS4 was obtained by reaction of TosNSCl2 (Tos = p-MeC6H4SO2) with Ph3CSH in CS2 in the presence of triethylamine. The reaction mechanism is discussed.
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    Anorganische Bi(cyclopentasilanyle): Synthese und spektroskopische Charakterisierung (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1517-1522 
    Details
    ISSN: 0044-2313
    Keywords: Bi(cyclopentasilanyls) ; hydrosilanes ; halosilanes ; 29Si-NMR, mass spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Inorganic Bi(cyclopentasilanyls): Synthesis and Spectroscopic CharacterizationNonachloro- or nonabromocyclopentasilane, which are accessible from nonaphenylcyclopentasilane with HX/AlX3 (X = Cl, Br), easily can be converted to the bicyclic oligosilanes bi(nonachlorocyclopentasilanyl) (7) and bi(nonabromocyclopentasilanyl) (8) upon treatment with (t-bu)2Hg. The phenylderivative bi(nonaphenylcyclopentasilanyl) (6) can be synthesized from bromononaphenylcyclopentasilane with naphthyllithium. The reaction of 6 with HX/AlX3 again affords 7 or 8. When 7 or 8 are reacted with LiAlH4, about 15% of cyclopentasilane are obtained along with the expected product bi(cyclopentasilanyl), what demonstrates the remarkable sensitivity of the central Si—Si-bond in 7 and 8 towards nucleophilic attack. A smaller binding energy of the central Si—Si-bond in 7 and 9, however, cannot be deduced from mass spectroscopic studies.
    Notes: Ausgehend von Nonachlor- bzw. Nonabromcyclopentasilan, die durch Abspaltung der Phenylgruppen in Nonaphenylcyclopentasilan mit HX/AlX3 (X = Cl, Br) zugänglich sind, gelingt durch Kopplung mit (t-bu)2Hg die Synthese der bicyclischen Oligosilane Bi(nonachlorcyclopentasilanyl) (7) und Bi(nonabromcyclopentasilanyl) (8). Bi(nonaphenylcyclopentasilanyl) (6), das mit HX/AlX3 ebenfalls in 7 oder 8 überführt werden kann, läßt sich aus Bromnonaphenylcyclopentasilan mit Naphthyllithium darstellen. Die Hydrierung von 7 und 8 mit LiAlH4 liefert neben dem erwarteten Bi(cyclopentasilanyl) etwa 15% Cyclopentasilan, was auf eine bemerkenswerte Labilität der zentralen Si—Si-Bindung gegenüber nucleophilen Reagenzien schließen läßt. Massenspektroskopische Untersuchungen ergeben keine Hinweise auf eine geringere Bindungsstärke der mittelständigen Si—Si-Bindung in 7 und 9.
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    URL: http://dx.doi.org/10.1002/zaac.19956210914
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    Neue ternäre Kupferpnictide mit modifizierten BaAl4-Strukturen (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1523-1530 
    Details
    ISSN: 0044-2313
    Keywords: Ternary copper pnictides ; alkaline earth ; europium ; crystal structure ; magnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Ternary Copper Pnictides with Modified BaAl4 Type StructuresEuCu2As2 (a = 4.215(1) Å, c = 10.185(2) Å) and EuCu2Sb2 (a = 4.504(1) Å, c = 10.824(2) Å) were prepared by heating (900°C) mixtures of CuCl and arsenic (antimony) with europium. The by-products were dissolved by dilute acetic acid. The arsenide crystallizes in the ThCr2Si2 type structure (I4/mmm; Z = 2) with holes in the copper arrangement, whereas the antimonide forms the CaBe2Ge2 type structure (P4/nmm; Z = 2). The stability ranges of both phases were determined by mixed crystal formation in accordance with EuCu2As2-xSbx. Magnetic measurements showed, that Europium is divalent and that the compounds order magnetically at low temperatures. BaCu2Sb2 (I4/mmm; a = 4.655(1) Å, c = 32.709(6) Å; Z = 6) was prepared by heating a mixture of binary antimonides of barium and copper in a melt of NaCl/KCl. The structure of this compound consists building elements of the CaBe2Ge2 and the ThCr2Si2 type structure. The already known compounds SrCu2As2 and BaCu2As2 were produced in a homogeneous form for the first time and their structures (ThCr2Si2 type) redetermined by means of single crystal X-ray methods.
    Notes: EuCu2As2 (a = 4,215(1) Å, c = 10,185(2) Å) und EuCu2Sb2 (a = 4,504(1) Å, c = 10,824(2) Å) wurden durch Erhitzen entsprechender Gemenge aus CuCl und Arsen bzw. Antimon mit Europium auf ca. 900°C dargestellt und mit verd. Essigsäure von den Nebenprodukten befreit. Das Arsenid kristallisiert im ThCr2Si2-Typ (I4/mmm; Z = 2) mit einer geringfügig unterbesetzten Cu-Punktlage, das Antimonid bildet dagegen die CaBe2Ge2-Struktur (P4/nmm; Z = 2). Durch Mischkristallbildung gemäß EuCu2As2-xSbx wurde das jeweilige Existenzgebiet der Randphasen ermittelt. Europium ist in beiden Verbindungen sowie im analogen Phosphid zweiwertig, die Substanzen ordnen bei tiefen Temperaturen magnetisch. BaCu2Sb2 (I4/mmm; a = 4,655(1) Å, c = 32,709(6) Å; Z = 6) konnte durch Umsetzung binärer Bariumantimonide mit Cu2Sb in einer NaCl/KCl-Schmelze bei 900°C erhalten werden. Die Struktur besteht aus Bauelementen der CaBe2Ge2-und ThCr2Si2-Struktur. Die bereits bekannten Verbindungen SrCu2As2 und BaCu2As2 wurden erstmals röntgenrein dargestellt und ihre Strukturparameter (ThCr2Si2-Typ) anhand von Einkristallen neu bestimmt.
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    Synthese und Kristallstruktur des Zirkonocen-Alkinyl-Alkenyl-Komplexes (Z)—Cp2Zr(C≡CPh){C(Ph) = C(H)P(SiMe3)2}Professor Wilhelm Preetz zum 60. Geburtstage gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1531-1534 
    Details
    ISSN: 0044-2313
    Keywords: Zirconocene alkynyl alkenyl complex ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of the Zirkonocene Alkynyl Alkenyl Complex (Z)—Cp2Zr(C≡CPh){C(Ph) = C(H)P(SiMe3)2}The reaction of (Z)—Cp2Zr(C(Ph) = C(H)P(SiMe3)2}(Cl) with lithium phenylacetylide yields the zirconocene alkynyl alkenyl complex (Z)—Cp2Zr(C≡CPh){C(Ph) = C(H)P(SiMe3)2} (1). 1 was characterised spectroscopically (IR, NMR, MS) and by X-ray structure determination. The complex crystallises triclinic in the space group P1 with a = 10.561(10), b = 11.226(12), c = 14.274(13) Å, α = 70.87(7), β = 77.70(7), γ = 77.85(7)°. In 1, there are two different Zr—C bond distances (Zr—C(=C) 2.415(6), Zr—C(≡C) 2.309(6) Å). A Zr—P interaction (Zr—P 2.774(3) Å) is observed in the solid state.
    Notes: Die Reaktion von (Z)—Cp2Zr{C(Ph) = C(H)P(SiMe3)2}(Cl) mit Lithiumphenylacetylid liefert den Zirkonocen-Alkinyl-Alkenyl-Komplex (Z)—Cp2Zr(C≡CPh){C(Ph) = C(H)P(SiMe3)2} (1). 1 wurde spektroskopisch (IR, NMR, MS) und röntgenstrukturanalytisch charakterisiert. Die Verbindung kristallisiert triklin in der Raumgruppe P1 mit a = 10,561(10), b = 11,226(12), c = 14,274(13) Å, α = 70,87(7), β = 77,70(7), γ = 77,85(7)°. 1 weist zwei unterschiedliche Zr—C-Bindungslängen auf (Zr—C(=C)) 2,415(6), Zr—C(≡C) 2,309(6) Å). Im Festkörper wird eine Zr—P-Wechselwirkung beobachtet (Zr—P 2,774(3) Å).
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    Nitrido-silicate. III. Hochtemperatur-Synthese, Kristallstruktur und magnetische Eigenschaften von Ce3[Si6N11] (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1535-1538 
    Details
    ISSN: 0044-2313
    Keywords: Silicon nitrides ; nitrido-silicates ; cerium ; crystal structure ; magnetic susceptibility ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitrido-silicates. III [1] High-Temperature Synthesis, Crystal Structure, and Magnetic Properties of Ce3[Si6N11]Pure Ce3[Si6N11] was obtained as transparent yellow crystals by reaction of metallic cerium with silicon diimide (Ce:Si = 1:2) under nitrogen atmosphere in a specially developed high-frequency furnace at 1660°C. Ce3[Si6N11] (P4bm, a = 1013.7(3), c = 483.9(5) pm, Z = 2, R = 0.034, wR = 0.024) contains Ce3+ ions as well as a three-dimensional covalent anionic network structure of corner-sharing SiN4 tetrahedra. Measurements of the magnetic susceptibility gave no indications for magnetic ordering phenomena in the temperature range between 2 and 300 K. Above 100 K pure Curie-Weiss behaviour (μeff = 2,10 μB, determined at room temperature) was observed.
    Notes: Transparent gelbe Kristalle von Ce3[Si6N11] wurden phasenrein durch Umsetzung von metallischem Cer mit Siliciumdiimid (Ce:Si = 1:2) unter Stickstoffatmosphäre in einem speziellen Hochfrequenzofen bei 1660°C synthetisiert. Ce3[Si6N11] (P4bm, a = 1013,7(3), c = 483,9(5) pm, Z = 2, R = 0,034, wR = 0,024) besteht im Festkörper aus Ce3+-Ionen sowie einer kovalenten, dreidimensional vernetzten Anionenteilstruktur eckenverknüpfter SiN4-Tetraeder. Messungen der magnetischen Suszeptibilität ergaben keine Hinweise auf magnetische Ordnungsphänomene im Temperaturbereich von 2 bis 300 K. Oberhalb 100 K wurde reines Curie-Weiss-Verhalten (μeff = 2,10 μB, ermittelt bei Raumtemperatur) beobachtet.
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    Die Reaktion von λ5-Diphospheten mit COS und CO2 Dihydro-λ5-PhospheteProfessor Hubert Schmidbaur zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1539-1546 
    Details
    ISSN: 0044-2313
    Keywords: 3-oxo-3,4-dihydro-1λ5-phosphete-2-yl ; 3-oxo-2,3-dihydro-1λ5-phosphete-2-yl ; nmr ; ir ; mass spectra ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of λ5-Diphosphetes with COS and CO2. Dihydro-λ5-Phosphetes1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphete, 1, reacts with COS to yield the (3-oxo-3,4-dihydro-1λ5-phosphete-2-yl)-phosphonothioic bis(dimethylamide) 7. Reaction of dimethyl substituted 1, i.e. 1,1,3,3-tetrakis(dimethylamino)-2,4-dimethyl-1λ5,3λ5-diphosphete 4, with COS and CO2 results in (3-oxo-2,3-dihydro-1λ5-phosphete-2-yl)-phosphonothioic bis(dimethylamide) 9, and (3-oxo-2,3-dihydro-1λ5-phosphete-2-yl)-phosphonic bis(dimethylamide) 10, respectively. Reaction mechanisms are suggested. 7, 9 and 10 are characterized by their properties, and their nmr, mass-, and ir-spectra. The results of X-ray structural analyses of 9 and 10 are reported and discussed.
    Notes: 1,1,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5-diphosphet, 1, reagiert mit COS zu (3-Oxo-3,4-dihydro-1λ5-phosphet-2-yl)-phosphonothiosäure-bis(dimethylamid) 7. Die Umsetzung von dimethylsubstituiertem 1, d. h. 1,1,3,3-Tetrakis(dimethylamino)-2,4-dimethyl-1λ5,3λ5-diphosphet 4 mit COS und CO2 führt zu (3-Oxo-2,3-dihydro-1λ5-phosphet-2-yl)-phosphonothiosäure-bis(dimehthylamid) 9 bzw. (3-Oxo-2,3-dihydro-1λ5-phosphet-2-yl)-phosphonsäure-bis(dimethylamid) 10. Es werden Reaktionsmechanismen vorgeschlagen. 7, 9 und 10 sind durch Eigenschaften und ihre NMR-, Massen- und IR-Spektren charakterisiert. Die Ergebnisse der Röntgenstrukturanalysen von 9 und 10 werden mitgeteilt und diskutiert.
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    Neue Alkylchlorsulfonium-Salze und Kristallstruktur von Diethylchlorsulfoni-umhexachloroantimonat (C2H5)2SCl+SbCl6- (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1547-1551 
    Details
    ISSN: 0044-2313
    Keywords: Dialkylchlorosulfonium hexachloroantimonates ; crystal structure ; preparation ; IR, Raman, NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Alkylchlorosulfonium Salts and Crystal Structure of Diethylchlorosulfonium-Hexachloroantimonate (C2H5)2SCl+SbCl6-We describe the preparation and spectroscopic characterization of Dialkylchlorosulfonium-Hexachloroantimonates R2SCl+SbCl6- (R = C2H5, i-C3H7) and the crystal structure of Diethylchlorosulfonium-Hexachloroantimonate (C2H5)2SCl+SbCl6- at 172(1) K. The salt crystallize in the orthorhombic space group P212121 with a = 980.4(13) pm, b = 1010.6(8) pm, c = 1492.8(14) pm with four formula units per unit cell.
    Notes: Es wird die Darstellung und spektroskopische Charakterisierung von Dialkylchlorsulfoniumhexachloroantimonaten R2SCl+SbCl6- (R = C2H5, i-C3H7), sowie die Einkristallröntgenstrukturanalyse von Diethylchlorsulfoniumhexachloroantimonat (C2H5)2SCl+SbCl6- bei 172(1) K beschrieben. Das Salz kristallisiert in der orthorhombischen Raumgruppe P212121 mit a = 980,4(13) pm, b = 1010,6(8) pm, c = 1492,8(14) pm mit 4 Formeleinheiten pro Elementarzelle.
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    Reaktion von Chlornitrat mit CF3I: Isolierung von Trifluormethylchloriodnitrat CF3I(Cl)ONO2 und Kristallstruktur von Trifluormethylioddinitrat CF3I(ONO2)2 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1552-1557 
    Details
    ISSN: 0044-2313
    Keywords: Chlorine Nitrate ; Trifluormethylchloroiodinenitrate ; Trifluormethyliodinedinitrate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Chlorine Nitrate with CF3I: Isolation of Trifluormethylchloroiodinenitrate CF3I(Cl)ONO2 and the Crystal Structure of Trifluormethyliodinedinitrate CF3I(ONO2)2CF3I reacts with ClONO2 to Iodine(III)-compounds. After an addition CF3I(Cl)ONO2 is isolated and characterized by vibrational spectra. With surplus ClONO2 it is formed CF3I(ONO2)2.CF3I(ONO2)2 crystallizes monoclinic in the space group P21/c with the cell parameters a = 1 024.3(6) pm, b = 873.5(6) pm, c = 873.4(6) pm and Z = 4.We measered following bonding distances: I—O: 207.3(3) and 220.8(2) pm, I—C: 221.1(4) pm and N—O: from 119.1(4) to 141.5(3) pm.Through an intermolecular I ··· O-contact the central iodine becomes a distorted plane geometry.
    Notes: CF3I reagiert mit ClONO2 in einer oxidativen Additionsreaktion zu Iod(III)-Verbindungen. Das Additionsprodukt CF3I(Cl)ONO2 wird isoliert und schwingungsspektroskopisch charaktersiert. Mit überschüssigem ClONO2 bildet sich CF3I(ONO2)2.CF3I(ONO2)2 kristallisiert monoklin in der Raumgruppe P21/c mit a = 1 024,3(6) pm, b = 873,5(6) pm, c = 873,4(6) pm und Z = 4.Es werden folgende Bindungslängen gemessen: I—O: 207,3(3) bzw. 220,8(2) pm, I—C: 221,2(4) pm und N—O: 119,1(4) bis 141,5(3) pm.Durch einen intermolekularen I ··· O-Kontakt erlangt das zentrale Iodatom eine verzerrt-planare Umgebung.
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    Osmium(II)-Phthalocyanine: Darstellung und Eigenschaften von Di(acido)phthalocyaninatoosmaten(II) (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1558-1566 
    Details
    ISSN: 0044-2313
    Keywords: Osmium(II) phthalocyanines ; cyclic voltammetry ; uv-vis spectra, vibrational spectra, 1H, 13C nmr spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Osmium(II) Phthalocyanines: Preparation and Properties of Di(acido)phthalocyaninatoosmates(II)“H[Os(X)2Pc2-]” (X = Br, Cl) reacts in basic medium or in the melt with (nBu4N)X forming less stable, diamagnetic, darkgreen (nBu4N)2[Os(X)2Pc2-]. Similar dicyano and diimidazolido(Im) complexes are formed by the reaction of “H[Os(Cl)2Pc2-]” with excess ligand in the presence of [BH4]-. The cyclic voltammograms show up to three quasireversible redoxprocesses: E1/2(I) = 0.13 V (X = CN), -0.03 V (Im), -0.13 V (Br) resp. -0.18 V (Cl) is metal directed (OsII/III), E1/2(II) = 0.69 V (Cl), 0.71 V (Br), 0.83 V (CN), 1.02 V (Im) is ligand directed (Pc2-/-) and E1/2(III) = 1.17 V (Cl) resp. 1.23 V (Br) is again metal directed (OsIII/IV). Between the typical “B” (∼16.2 kK) and “Q” (∼29.4 kK), “N regions” (∼34.1 kK) up to seven strong “extra bands” of the phthalocyanine dianion (Pc2-) are observed in the uv-vis spectrum. Within the row CN 〉 Im 〉 Br 〉 Cl, most of the bands are shifted slightly, the “extra bands” considerably more to lower energy in correlation with E1/2(I). The vibrational spectra are typical for the Pc2- ligand with D4h symmetry. M.i.r. bands at 514, 909, 1 173 and 1 331 cm-1 are specific for hexa-coordinated low spin OsII phthalocyanines. In the resonance Raman (r.r.) spectra polarized, depolarized or anomalously polarized deformation and stretching vibrations of the Pc2- ligand will be selectively enhanced, if the excitation frequency coincides with “extra bands”. With excitation at ∼19.5 kK the intensity of the symmetrical Os—X stretching vibration at 295 cm-1 (X = Cl), 252 cm-1 (X = Im) and 181 cm-1 (X = Br) is r.r. enhanced, too. The asymmetrical Os—X stretching vibration is observed in the f.i.r. spectrum at 345 cm-1 (X = CN), 274 cm-1 (X = Cl), 261 cm-1 (X = Im) and 200 cm-1 (X = Br).
    Notes: “H[Os(X)2Pc2-]” (X = Br, Cl) reagiert in basischer Lösung oder in der Schmelze mit (nBu4N)X zu luftempfindlichem, diamagnetischem, dunkelgrünem (nBu4N)2[Os(X)2 · Pc2-]. Die entsprechenden Dicyano- und Diimidazolido(Im)-Komplexe bilden sich aus “H[Os(Cl)2Pc2-]” bei Ligandüberschuß in Gegenwart von [BH4]-. Die Zyklovoltammogramme zeigen bis zu drei quasireversible Redoxprozesse: E1/2(I) = 0,13 V (X = CN), -0,03 V (Im), -0,13 V (Br) bzw. -0,18 V (Cl) ist metallgerichtet (OsII/III), E1/2(II) = 0,69 V (Cl), 0,71 V (Br), 0,83 V (CN), 1,02 V (Im) ist ligandgerichtet (Pc2-/-) und E1/2(III) = 1,17 V (Cl) bzw. 1,23 V (Br) ist wiederum metallgerichtet (OsIII/IV). Im UV-Vis-NIR-Spektrum treten zwischen den typischen “B-” (∼16,2 kK) und “Q-” (∼29,4 kK), “N-Bereichen” (∼34,1 kK) bis zu sieben intensive “Extrabanden” des Phthalocyanin-Dianions (Pc2-) auf. Die meisten Banden verschieben sich in der Reihe CN 〉 Im 〉 Br 〉 Cl in Korrelation mit E1/2(I) geringfügig, die “Extrabanden” deutlich stärker zu niedriger Energie. Die Schwingungsspektren sind für den Pc2--Liganden mit D4h-Symmetrie kennzeichnend. MIR-Banden bei 514, 909, 1 173 und 1 331 cm-1 sind spezifisch für hexakoordinierte low spin OsII-Phthalocyanine. In den Resonanz-Raman(RR)Spektren werden je nach Anregungsfrequenz im Bereich der “Extrabanden” entweder die polarisierten, depolarisierten oder anomal polarisierten Deformations- und Valenzschwingungen des Pc2--Liganden angeregt. Mit Anregungsfrequenzen um 19,5 kK wird darüber hinaus die Intensität der totalsymmetrischen (Os—X)-Valenzschwingung bei 295 cm-1 (X = Cl), 252 cm-1 (X = Im) und 181 cm-1 (X = Br) selektiv durch den RR-Effekt verstärkt. Die asymmetrische (Os—X)-Valenzschwingung erscheint im FIR-Spektrum bei 345 cm-1 (X = CN), 274 cm-1 (X = Cl), 261 cm-1 (X = Im) und 200 cm-1 (X = Br).
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    Kristallstrukturbestimmungen an vier monoklinen Weberiten Na2MIIMIIIF7 (MII = Fe, Co; MIII = V, Cr) (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1573-1581 
    Details
    ISSN: 0044-2313
    Keywords: Weberite structure ; structure determination ; di-sodium iron vanadium hepta-fluoride ; di-sodium iron chromium hepta-fluoride ; di-sodium cobalt vanadium hepta-fluoride ; disodium cobalt chromium hepta-fluoride ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure Determinations of Four Monoclinic Weberites Na2MIIMIIIF7 (MII = Fe, Co; MIII = V, Cr)By solid state reaction of the binary fluorides single crystals of the following weberites were prepared and their monoclinic structure (space group C2/c, Z = 16) determined by X-ray methods: Na2FeVF7 (a = 1 271.0(3), b = 742.9(1), c = 2 471.6(5) pm, β = 100.03(3)°; R1 = 0.043 (1 545 Reflexe); Fe—F = 203.8, V—F = 193.0 pm); Na2FeCrF7 (a = 1 262.5(3), b = 739.1(1), c = 2 460.5(5) pm, β = 99.93(3)°; R1 = 0.029 (2 340); Fe—F = 203.6, Cr—F = 190.5 pm); Na2CoVF7 (a = 1 270.3(5), b = 739.1(3), c = 2 465.1(10) pm, β = 100.02(3)°; R1 = 0.028 (2 250); Co—F = 201.6, V—F = 193.6 pm); Na2CoCrF7 (a = 1 257.8(3), b = 733.5(1), c = 2 441.5(5) pm, β = 99.64(3)°; R1 = 0.030 (2 227); Co—F = 201.2, Cr—F = 190.2 pm). Concerning the above average distances within the distorted [MF6] octahedra and the shape of [NaF8] coordination details are given and discussed.
    Notes: Durch Festkörperreaktion der binären Fluoride wurden Einkristalle der folgenden Weberite dargestellt und röntgenographisch deren monokline Struktur bestimmt (Raumgruppe C2/c, Z = 16): Na2FeVF7 (a = 1 271,0(3), b = 742,9(1), c = 2 471,6(5) pm, β = 100,03(3)°; R1 = 0,043 (1 545 Reflexe); Fe—F = 203,8, V—F = 193,0 pm); Na2FeCrF7 (a = 1 262,5(3), b = 739,1(1), c = 2 460,5(5) pm, β = 99,93(3)°; R1 = 0,029 (2 340); Fe—F = 203,6, Cr—F = 190,5 pm); Na2CoVF7 (a = 1 270,3(5), b = 739,1(3), c = 2 465,1(10) pm, β = 100,02(3)°; R1 = 0,028 (2 250); Co—F = 201,6, V—F = 193,6 pm); Na2CoCrF7 (a = 1 257,8(3), b = 733,5(1), c = 2 441,5(5) pm, β = 99,64(3)°; R1 = 0,030 (2 227); Co—F = 201,2, Cr—F = 190,2 pm). Zu den genannten mittleren Abständen in den verzerrten [MF6]-Oktaedern und zur Form der [NaF8]-Koordination werden Einzelheiten mitgeteilt und diskutiert.
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    [Mg3Cl5(Et2O)6]+: Darstellung, Strukturbestimmung und ab-initio-UntersuchungenProfessor Peter Paetzold zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1582-1588 
    Details
    ISSN: 0044-2313
    Keywords: [Mg3Cl5(Et2O)6] cation ; X-ray structure ; ab-initio calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Mg3Cl5(Et2O)6]+: Synthesis, Structure, and Ab-Initio CalculationsThe cation [Mg3Cl5(Et2O)6]+ of a chlorogallat has been prepared in a reaction of Ga2Cl4 with MgCp2* and was characterized by a X-ray single-crystal structure analysis. For understanding of the conditions of formation of neutral and charged magnesium chlorids and of the processes in the complex reaction system ab-initio calculations were performed.
    Notes: Das Kation [Mg3Cl5(Et2O)6]+ eines Chlorogallats wurde im Rahmen einer Umsetzung von Ga2Cl4 mit MgCp2* dargestellt und durch eine Kristallstrukturbestimmung röntgenographisch charakterisiert. Um die Bildungsbedingungen von neutralen und ionischen Magnesiumchloriden und die komplexen Reaktionsabläufe im Synthesegemisch zu verstehen, wurden quantenchemische ab-initio-Rechnungen angefertigt.
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    Ruthenium(III)-Phthalocyanine: Darstelllung und Eigenschaften von Di(halogeno)phthalocyaninato(1-)ruthenium(III), [Ru(X)2Pc] (X = Cl, Br, I) (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1567-1572 
    Details
    ISSN: 0044-2313
    Keywords: Ruthenium(III) phthalocyanines ; phthalocyanine(1-) anion ; optical spectra ; vibrational spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ruthenium(III) Phthalocyanines: Synthesis and Properties of Di(halo)phthalocyaninato(1-)ruthenium(III)Di(halo)phthalocyaninato(1-)ruthenium(III), [Ru(X)2Pc-] (X = Cl, Br, I) is prepared by oxidation of [Ru(X)2Pc2-]- (Cl, Br, OH) with halogene in dichloromethane. The magnetic moment of [Ru(X)2Pc-] is 2,48 μB (X = Cl) resp. 2,56 μB (X = Br) in accordance with a systeme of two independent spins (low spin RuIII and Pc-: S = 1/2). The optical spectra of the red violet solution of [Ru(X)2Pc-] (Cl, Br) are typical for the Pc- ligand with the “B” at 13.5 kK, “Q1” at 19.3 kK and “Q2 region” at 31.9 kK. Sytematic spectral changes within the iron group are discussed. The presence of the Pc- ligand is confirmed by the vibrational spectra, too. Characteristic are the metal dependent bands in the m.i.r. spectra at 1 352 and 1 458 cm-1 and the strong Raman line at 1 600 cm-1. The antisymmetric Ru—X stretch (vas(Ru—X)) is observed at 189 cm-1 (X = I) resp. 234 cm-1 (X = Br). There are two interdependent bands at 295 and 327 cm-1 in the region expected for vas(Ru—Cl) attributed to strong interaction of vas(Ru—Cl) with an out-of-plane Pc- tilting mode of the same irreducible representation. Only the symmetric Ru—Br stretch at 183 cm-1 is selectively enhanced in the resonance-Raman(RR) spectra. The Raman line at 168 cm-1 of the diiodo complex is assigned to loosely bound iodine. The broad band at 978 cm-1 in the RR spectra of the dichloro complex is due to an intraconfigurational transition within the electronic ground state of low spin RuIII split by spin orbit coupling.
    Notes: Di(halogeno)phthalocyaninato(1-)ruthenium(III), [Ru(X)2Pc-] (X = Cl, Br, I) wird durch Oxydation von [Ru(X)2Pc2-]- (Cl, Br, OH) mittels Halogen in Dichlormethan dargestellt. Übereinstimmend mit einem System zweier unabhängiger Spins (low-spin RuIII und Pc-: S = 1/2) beträgt das magnetische Moment von [Ru(X)2Pc-] 2,48 (X = Cl) bzw. 2,56 μB (X = Br). Die optischen Spektren von in Lösung rotviolettem [Ru(X)2Pc-] (X = Cl, Br) sind typisch für den Pc--Liganden mit dem “B-” bei 13,5 kK, “Q1-” bei 19,3 kK und “Q2-Bereich” bei 31,9 kK. Die systematischen Änderungen des optischen Spektrums innerhalb der Eisengruppe werden diskutiert. Die Präsenz des Pc--Liganden wird ebenfalls durch die Schwingungsspektren bestätigt. Charakteristisch sind die metallabhängigen Banden bei 1 352 und 1 458 cm-1 im MIR-Spektrum sowie die intensive Raman-Linie bei 1 600 cm-1. Die antisymmetrische Ru—X-Valenzschwingung (vas(Ru—X)) liegt bei 189 cm-1 (X = I) bzw. 234 cm-1 (X = Br). Im Erwartungsbereich von vas(Ru—Cl) treten zwei voneinander abhängige Banden bei 295 und 327 cm-1 auf, die auf der Kopplung von vas(Ru—Cl) mit einer Aus-der-Ebene-Pc--Deformationsschwingung gleicher Rasse beruhen. In den Resonanz-Raman(RR)-Spektren wird nur die symmetrische Ru—Br-Valenzschwingung bei 183 cm-1 selektiv verstärkt. Die Raman-Linie bei 168 cm-1 für den Diiodo-Komplex wird angelagertem Iod zugeordnet. Die RR-Spektren des Dichloro-Komplexes weisen den aus der Aufspaltung des elektronischen Grundzustandes von low-spin RuIII durch Spin-Bahn-Kopplung resultierenden Intrakonfigurationsübergang bei 978 cm-1 auf.
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    Struktur und ausgewählte Reaktionen von ReCl4(PPh3)2 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1797-1799 
    Details
    ISSN: 0044-2313
    Keywords: Tetrachloro-bis(triphenylphosphane)rhenium(IV) ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: ReCl4(PPh3)2 - Reactions and StructureThe compounds ReCl4(PPh3)2 and Re2OCl3(C2H5COO)2(PPh3)2 resulting from the reaction of ReOCl3(PPh3)2 with PPh3 in boiling propionic acid and HCl atmosphere were characterized by their VIS-spectra and structural data.Ligand exchange reactions with acetylacetone gave ReCl2(acac)2 as well as ReCl2(acac)(PPh3)2.Crystallographic data see “Inhaltsübersicht”.
    Notes: Die bei der Umsetzung von ReOCl3(PPh3)2 mit PPh3 in siedender Propionsäure unter HCl nebeneinander entstehenden Verbindungen ReCl4(PPh3)2 und Re2OCl3(C2H5COO)2(PPh3)2 wurden spektroskopisch und röntgenographisch charakterisiert. Bei Ligandenaustauschreaktionen mit Acetylaceton wurden sowohl ReCl2(acac)2 als auch ReCl2(acac)(PPh3)2 identifiziert.ReCl4(PPh3)2: Raumgruppe P21/n; Z = 2; 2 908 beobachtete unabhängige Reflexe; R = 0,0322; Gitterabmessungen bei 210 K: a = 9,324(4) Å; b = 20,93(1) Å; c = 9,636(4) Å; β = 117,66(1)°.
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    Trimethylstannyl- und Dimethylstannyl-substituierte Pyrrole - Synthesen, Spektren und Strukturen (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1785-1796 
    Details
    ISSN: 0044-2313
    Keywords: Organotin pyrrole derivatives ; NMR, vibrational spectra, X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trimethylstannyl- and Dimethylstannyl-substituted Pyrroles - Synthesis, Spectra, and StructuresMonomeric trimethylstannyl pyrroles, Me3Sn—R (Me = CH3 and R = —NC4H4, —NC4H2Me2-2,5, —NC4Me4-2,3,4,5, —C4H3NMe-1), are synthesized by metathesis reactions from Me3SnCl with 1(N)- and 2(C)-lithium pyrroles, respectively. An almost similar procedure gives monomeric dimethylstannylbis(pyrroles), Me2SnR2 (1 a - 3 a), from Me2SnCl2 and 1-Li-pyrrolides (1 : 2 molar ratio) in good yields. Lithiated 1,2,5-trimethylpyrrole and Me3SnCl forms the compound Me3Sn—CH2—C4H2Me(-5)NMe (8), the reaction of Me2SnCl2 with 2-lithium-1-methylpyrrole gives oligomeric [Me2Sn—C4H2NMe—]x, (6 a). The mass-, NMR, and vibrational spectra have been measured and discussed. The results of the X-ray structure determinations of Me3Sn—NC4H4 (1) and Me2Sn(—NC4Me4)2 (3 a) are compared with the structures of the known dimethylmetal pyrroles of Al, Ga, and In.
    Notes: Monomere Trimethylstannylpyrrole, Me3Sn—R (Me = CH3, R = —NC4H4, —NC4H2Me2-2,5, —NC4Me4-2,3,4,5, —C4H3NMe-1), werden durch Metathese aus Me3SnCl und 1(N)- bzw. 2(C)-lithiierten Pyrrolen synthetisiert. Analog hierzu werden aus Me2SnCl2 und Li—N Pyrroliden (Molverhältnis 1 : 2) die ebenfalls monomeren Dimethylstannylbis(pyrrole), Me2SnR2 (1a - 3a), in guten Ausbeuten erhalten. Einfach lithiiertes 1,2,5-Trimethylpyrrol bildet mit Me3SnCl die Verbindung Me3Sn—CH2—C4H2Me(-5)NMe (8); die Umsetzung von Me2SnCl2 mit 2C-lithiiertem 1-Methylpyrrol ergibt oligomeres [Me2Sn—C4H2NMe—]x (6 a). Die Massen-, Kernresonanz- und Schwingungsspektren werden aufgenommen und diskutiert. Die Ergebnisse der Röntgeneinkristallstrukturanalysen von Me3Sn—NC4H4 (1) und Me2Sn(—NC4Me4)2 (3 a) werden mit den Strukturdaten der bekannten Dimethylmetallpyrrole des Al, Ga und In Verglichen.
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    Sulfur-Selenium Chelates: Crystal structure of the first titanocene derivative Ti(η5-C5H5)2SSe4 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1800-1802 
    Details
    ISSN: 0044-2313
    Keywords: Titanocene sulfidotetraselenides ; Selenium-sulfur chelates ; X-ray analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Schwefel-Selen Chelate: Kristallstruktur des ersten Titanocenderivats Ti(η5-C5H5)2SSe4Die Kristallstruktur von Bis(→5-cyclopentadientyl)titana(TiIV)-thiacyclohexaselenan, Ti(η5-C5H5)2SSe4 (1) wurde durch Röntgenstrukturanalyse bestimmt. (1) kristallisiert monoklin in der Raumgruppe P21/c, Z = 4, a = 13,179, b = 8,087, c = 14,447 Å, β = 114,857°. Der sechsgliedrige Heterocyclus TiSSe4 hat die erwartete Sesselkonformation. Im Chelatring ist das Ti-Atom and S und Se gebunden. Die Geometrie von (1) stimmt sehr gut mit der von Ti(η5-C5H5)2Se5 überein.
    Notes: The crystal structure of bis(η5-cyclopentadienyl)titana(TiIV)-thiacyclohexaselenane, Ti(η5-C5H5)2SSe4 (1), has been determined by X-ray diffraction data. (1) crystallizes in the monoclinic space group P21/c with four formula units in the unit cell. The cell dimensions are a = 13.179, b = 8.087, c = 14.447 Å, β = 114.857°. The six-membered heterocycle TiSSe4 has the expected chair conformation. In the chelate ring the Ti atom is S- and Se-bonded. The geometry of (1) corresponds closely to that of Ti(→5-C5H5)2Se5.
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    Silicate und Germanate mit der Struktur des Silicocarnotits (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1803-1807 
    Details
    ISSN: 0044-2313
    Keywords: Silicates ; germanates ; silicocarnotite structure type ; apatites ; lanthanoid compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Silicates and Germanates with the Structure of SilicocarnotiteA number of lanthanoid-containing compounds Ca3Ln2(XO4)3 with X = Si, Ge have been prepared, which have the silicocarnotite structure. With the silicates, Ln ranges from Sm to Lu, with the germanates only from Sm to Tb. Ca3Y2(SiO4)3 crystallizes in this structure type, too. In the case of Ln = La—Nd, mixtures “Ca3Ln2(XO4)3” are formed containing apatite phases. The germanates Ca3Ln2(GeO4)3 with Ln = Dy—Lu; Y, Sc and Ca3Sc2(SiO4)3 have the garnet structure, as already known.In addition, the lead compounds Pb3La2(SiO4)3, Pb3Y2(SiO4)3 and Pb2Y3(SiO4)3O0,5 have been synthesized. They have an apatite structure where the halogen positions are unoccupied or half-occupied.
    Notes: Dargestellt wurde eine Reihe von Lanthanoid-haltigen Verbindungen Ca3Ln2(XO4)3 mit X = Si, Ge, welche die Struktur des Silicocarnotits aufweisen. Bei den Silicaten erstreckt sich Ln von Sm bis Lu, bei den Germanaten nur von Sm bis Tb. Außerdem kristallisiert Ca3Y2(SiO4)3 in diesem Strukturtyp. Im Falle von Ln = La — Nd liegen Gemische “Ca3Ln2(XO4)3” unter Beteiligung von Apatitphasen vor. Die Germanate Ca3Ln2(GeO4)3 mit Ln = Dy—Lu; Y, Sc haben, wie bereits bekannt, Granatstruktur, ebenso Ca3Sc2(SiO4)3.Zusätzlich wurden die Bleiverbindungen Pb3La2(SiO4)3, Pb3Y2(SiO4)3 sowie Pb2Y3(SiO4)3O0,5 dargestellt, die eine Apatitstruktur mit nichtbesetzten bzw. hälftig besetzten Halogenlagen haben.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/zaac.19956211101
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    Untersuchungen zur thermischen Zersetzung der Ammoniumyttriumhalogenide II. Ammoniumyttriumiodid (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1808-1812 
    Details
    ISSN: 0044-2313
    Keywords: Ammonium Yttrium Iodide ; thermal decomposition ; thermochemical data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigation on the Thermal Decomposition of Ammonium Yttrium Halides II. Ammonium Yttrium Iodide(NH4)3YI6 decomposes directly into YI3,s NH3,g and HI,g. In connection with the thermal decomposition of NH4I the decomposition-pressure-function is given and the enthalpy of formation and the standard entropy of the phases are derived.
    Notes: Die thermische Zersetzung des Ammoniumyttriumiodides (NH4)3YI6 erfolgt direkt in YI3,f, NH3,g und HI,g. Im Anschluß an die thermische Zersetzung von NH4I werden die Zersetzungsdruckfunktionen dargestellt und die Bildungsenthalpien und Standardentropien der Phasen hergeleitet.
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    The Preparation and X-Ray Structure of [AsPh4][Ph2P(S)NSiMe3] · 0.5 THFDedicated to Professor Herbert W. Roesky on the Occasion of his 60th Birthday (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1813-1817 
    Details
    ISSN: 0044-2313
    Keywords: [AsPh4][Ph2P(S)NSiMe3] · 0.5 THF ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Röntgen-Strukturbestimmung von [AsPh4][Ph2P(S)NSiMe3] · 0,5 THFDie Reaktion von Ph2P(S)N(SiMe3)2 mit Kalium-tert-butoxid im molaren Verhältnis 1:1 ergibt K[Ph2P(S)NSiMe3], das mit [AsPh4]Cl zum AsPh4+-Salz umgesetzt wird. Die Kristallstruktur von [AsPh4][Ph2P(S)NSiMe3] ·0,5 THF besteht aus AsPh4+ und Ph2P(S)NSiMe3- mit d(P—S) = 1,980(4) Å und d(P—N) = 1,555(8) Å. Der P—N—Si-Winkel im Anion beträgt 136,3(5)°. Der elektrophile Angriff von Ph2P(S)Cl erfolgt am Schwefel des Ph2P(S)NSiMe3-. Die Oxidation des Anions mit Iod ergibt ein Disulfid, das bei Umsetzung mit Kalium-tert-butoxid wieder K[Ph2P(S)NSiMe2] ergibt.
    Notes: The reaction of Ph2P(S)N(SiMe3)2 with potassium tert-butoxide in a 1:1 molar ratio produces K[Ph2P(S)NSiMe3], which was converted to the AsPh4+ salt by metathesis with [AsPh4]Cl. The X-ray crystal structure of [AsPh4][Ph2P(S)NSiMe3] · 0.5 THF consists of noninteracting AsPh4+ and Ph2P(S)NSiMe3- ions with d(P—S) = 1.980(4) Å and d(P—N) = 1.555(8) Å. The PNSi bite angle in the anion is 136.3(5)°. Electrophilic attack by Ph2P(S)Cl occurs at the sulfur atom of Ph2P(S)NSiMe3-. The oxidation of the anion with iodine produces a disulfide which regenerates K[Ph2P(S)NSiMe2] upon treatment with potassium tert-butoxide.
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    Zur kristallchemischen Ähnlichkeit von Aurid- und Halogenid-IonenProfessor Herbert W. Roesky zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1907-1912 
    Details
    ISSN: 0044-2313
    Keywords: Aurides ; anti perovskites ; alkali metal halide oxides ; K3BrO, K3IO, K3AuO, Rb3BrO, Rb3IO, Rb3AuO, Cs3BrO, Cs3IO, Cs3AuO ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Chemical Similarity of Auride and Halide AnionsThe crystallographic properties of the aurides M3AuO and the alkalimetal halide oxides M3XO (M = K, Rb, Cs; × = Br, I) are compared. Rb3BrO, Rb3IO, Cs3BrO, and Cs3IO have been prepared and characterized for the first time: Rb3BrO (a = 5.465(1) Å) crystallizes as a cubic anti perovskite, Cs3BrO (a = 7.800(6), c = 7.122(6) Å) and Cs3IO (a = 8.056(3), c = 7.168(3) Å) as hexagonal anti perovskites, Rb3IO (a = 7.889(1), c = 19.640(1) Å) as a hexagonal anti BaTiO3 type. The analysis of bond lengths, molar volumes and the systematic of the crystal structures leeds to the conclusion, that the crystallographic properties of auride- and bromide anions are similar. The radius of the Au- has been found to be 2.2 Å (KZ 12).
    Notes: Verglichen werden die kristallographischen Eigenschaften der Auride M3AuO und der Alkalimetallhalogenidoxide M3XO (M = K, Rb, Cs; × = Br, I). Rb3BrO, Rb3IO, Cs3BrO und Cs3IO werden erstmals dargestellt und strukturell charakterisiert: Rb3BrO (a = 5,465(1) Å) kristallisiert als kubischer anti-Perowskit, Cs3BrO (a = 7,800(6), c = 7,122(6) Å) und Cs3IO (a = 8,056(3), c = 7,168(3) Å) als hexagonale anti-Perowskite, Rb3IO (a = 7,889(1), c = 19,640(1) Å) im hexagonalen anti-BaTiO3-Typ. Die Analyse der Bindungsabstände und Molvolumina sowie die Systematik der Kristallstrukturen der Verbindungen M3YO (M = K, Rb, Cs; Y = Br, I, Au) belegen die kristallchemische Ähnlichkeit von Aurid- und Bromid-Ionen. Der Wirkungsradius des Au--Ions kann zu 2,2 Å (KZ 12) abgeschätzt werden.
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    A novel mononuclear gold(I) complex: Synthesis and x-ray structure of [Au{P(C6H5)3}3][SiF5] · 1.5 CH2Cl2Dedicated to Professor Herbert W. Roesky on the Occasion of his 60th Birthday (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1929-1932 
    Details
    ISSN: 0044-2313
    Keywords: Tris(triphenylphosphine)gold(I)-pentafluorosilicate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ein neuer einkerniger Gold(I)-Komplex: Synthese und Röntgen-Struktur von [Au{P(C6H5)3}3][SiF5] · 1,5 CH2Cl2Tris(triphenylphosphan)gold(I)-pentafluorosilicat ([Au{P(C6H5)3}3][SiF5]) wurde dargestellt und durch eine Einkristallstrukturanalyse charakterisiert. Der Komplex kristallisiert triklin, Raumtemperatur P1 (Nr. 2) mit a = 14,634(2) Å, b = 17,180(2) Å, c = 22,212(3) Å, α = 86,48(1)°, β = 78,95(1)°, γ = 83,99(1)°, Z = 4. Die Goldatome sind von je drei Triphenylphosphin-Liganden koordiniert zum trigonal-planaren [Au{P(C6H5)3}3]+-Kation. Getrennt davon liegt das trigonal-bipyramidale Anion [SiF5]- vor. Zwischen den Fluor- und Goldatomen wird keine Wechselwirkung beobachtet.
    Notes: Tris(triphenylphosphine)gold(I)-pentafluorosilicate(IV) ([Au{P(C6H5)3}3][SiF5]) was prepared and the structure was determined by single crystal x-ray diffraction. The complex crystallizes in the triclinic space group P1 (No. 2). The lattice constants are a = 14.634(2) Å, b = 17.180(2) Å, c = 22.212(3) Å, α = 86.48(1)°, β = 78.95(1)°, γ = 83.99(1)°. Number of molecules per cell: Z = 4. The gold atoms are coordinated to three triphenylphosphine ligands to form the trigonal planar cation [Au{P(C6H5)3}3]+. Separated from the cation is the [SiF5]- anion which is regular trigonal bipyramidal coordinated. No interactions between the fluorine atoms and the gold atoms were observed.
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    Polyol-Metall-Komplexe. X. Blei(II)-meso-oxolan-3,4-diolat(2-)-Monohydrat - ein polymeres Blei-alkoxid aus wäßriger Lösung (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 19-22 
    Details
    ISSN: 0044-2313
    Keywords: Lead ; meso-Oxolane-3,4-diolate(2-) ; Anhydroerythritol ; Coordination Polymer ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polyol Metal Complexes. X. Lead(II) meso-Oxolane-3,4-diolate(2-) Monohydrate - a Polymeric Lead Alkoxide from Aqueous SolutionIn the colourless crystals of Pb(C4H6O3) · H2O (P21/c, a = 569.8(3), b = 607.6(4), c = 1856.9(9) pm, β = 89.90(4)°, V = 642.9(6) · 106 pm3, Z = 4), lead(II)- and meso-oxolane-3,4-diolate(2-) ions form a one-dimensional coordination polymer; PbII is coordinated with four bridging alkoxide O-atoms (mean distance: 234.5 pm); some 100 pm more distant two μ-O-atoms of water molecules coordinate the lead ion.
    Notes: Blei(II)- und meso-Oxolan-3,4-diolat(2-)-Ionen bauen in den farblosen Kristallen von Pb(C4H6O3) · H2O (P21/c, a = 569,8(3), b = 607,6(4), c = 1856,9(9) pm, β = 89,90(4)°, V = 642,9(6) · 106 pm3, Z = 4) ein kettenförmiges Koordinationspolymer auf, in dem PbII von vier verbrückenden Alkoxid-O-Atomen koordiniert ist (mittlerer Abstand: 234,5 pm); ungefähr 100 pm weiter entfernt koordinieren zwei ebenfalls verbrückende Wasser-O-Atome.
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    Ein neues Oxophosphat (IV/III)-Anion - Darstellung und Kristallstruktur von Na6P4O10 · 2 H2O (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 7-13 
    Details
    ISSN: 0044-2313
    Keywords: Sodium phosphate ; oxophosphate (IV/III) ; crystal structure ; 31P-NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Oxophosphate (IV/III) Anion - Preparation and Crystal Structure of Na6P4O10 · 2 H2OA new oxophosphate anion, P4O106-, was obtained by cleavage and simultaneous oxidation of the cyclo-hexaphosphate(III) anion in a solution of aqueous ammonia and ethanol. With sodium it forms a salt with the composition Na6P4O10 · 2 H2O. The crystal structure has been determined by single crystal X-ray diffraction (3 745 diffractometer data), the cell constants were obtained from X-ray powder data, space group P1; a = 6.004(1), b = 6.173(2), c = 11.496(2) Å, α = 99.26(2)°, β = 95.92(2)°, γ = 117.63(2)°, Z = 1, R = 0.044. The backbone of the anion is formed by phosphorus atoms directly bonded to each other. The coordination of each phosphorus atom is completed to four by oxygene. The resulting oxidation numbers are +III for the inner phosphorus atoms and +IV for the terminal phosphorus atoms. The site symmetry of the anion is approximately C2h. Based on a 31P-NMR spectra of a solution the coupling constants of the AA ‘BB’ system were determined.
    Notes: Ein neues Oxophosphation, P4O106-, wurde durch oxidative Ringspaltung an cyclo-Hexaphosphaten(III) in ammoniakalisch/ethanolischer Lösung erhalten und die Struktur von Na6P4O10 · 2 H2O [Vierkreisdiffraktometerdaten (3 745 unabhängige Strukturfaktoren)] gelöst. Raumgruppe P1; a = 6,004(1); b = 6,173(2); c = 11,496(2) Å; α = 99,26(2)° β = 95,92(2)°; γ = 117,63(2)°; Z = 1; R = 0,044. Das „Rückgrat“ des kettenförmigen Anions sind vier verbundene Phosphoratome, deren Koordination mit Sauerstoff auf vier aufgefüllt wird. Dem entspricht die Oxidationsstufe +III für die inneren bzw. +IV für die terminalen Phosphoratome. Für das komplexe Anion ist die Punktsymmetrie C2h näherungsweise erfüllt. Aus 31P-NMR-Daten in Lösung wurden die vier Kopplungskonstanten des AA ‘BB’-Systems durch Spektrensimulation ermittelt.
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    Variable temperature 1H, 23Na, and 29Si MAS NMR studies on sodium silicate hydrates of composition Na2O · SiO2 · nH2O (n = 9, 6, 5): Local structure in crystals, melts, supercooled melts, and glasses (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 301-310 
    Details
    ISSN: 0044-2313
    Keywords: Solid-state NMR, 29Si, 1H, 23Na ; sodium silicate hydrates ; glass formation ; melting process ; structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Temperaturvariable 1H-, 23Na- und 29Si-MAS-NMR Untersuchungen an Natriumsilicathydraten der Zusammensetzung Na2O · SiO2 · nH2O (n = 9, 6, 5): Lokalstruktur in Kristallen, Schmelzen, unterkühlten Schmelzen und GläsernDie Lokalstruktur in Kristallen, Schmelzen, unterkühlten Schmelzen und Gläsern von Natriumsilicathydraten der Zusammensetzung Na2O · SiO2 · nH2O (n = 9, 6, 5) wird mittels temperaturvariabler 1H-, 23Na- und 29Si-MAS-NMR-Spektroskopie charakterisiert. Detaillierte in-situ Untersuchungen des Schmelzprozesses der kristallinen Hydrate zeigen die Bedeutung der Beweglichkeit der Wassermoleküle für den Schmelzmechanismus. In Abhängigkeit von der lokalen Umgebung zeigen kristallographisch unterschiedliche Natriumpositionen ein unterschiedliches Verhalten während des Schmelzprozesses. Die monomeren Silicatanionen der kristallinen Hydrate kondensieren während des Schmelzens zu oligomeren Anionen. Bei Abkühlung der Schmelzen tritt keine Rekristallisation, sondern Glasbildung auf, wenn die Schmelzen zuvor ca. 10 K über den Schmelzpunkt erhitzt werden. Wie in den Schmelzen werden in den Gläsern ebenfalls oligomere Silicatanionen beobachtet, die jedoch einen erhöhten Anteil an cyclotrimeren Spezies enthalten. Durch Kombination von in-situ MAS-NMR-Untersuchungen und Messungen der elektrischen Leitfähigkeit an den Schmelzen, unterkühlten Schmelzen und Gläsern wird eine Aufteilung in drei Temperaturbereiche vorgeschlagen, die durch Unterschiede in der Lokalstruktur und Dynamik der Natriumkationen, Wassermoleküle und Silicatanionen charakterisiert sind. Diese Bereiche umfassen einen Glas- und Transformationsbereich A bei tiefer Temperatur, einen Aggregationsbereich B bei mittleren Temperaturen und einen Lösungs- bzw. Elektrolytbereich C bei höheren Temperaturen. Im Bereich B wird eine Aggregation von hydratisierten Natriumkationen zu höheren Polykationenkomplexen angenommen, deren Beweglichkeit sich deutlich von der der Silicatanionen unterscheidet. Eine Bildung von langlebigen Kontaktionenpaaren zwischen Natriumkationen und Silicatanionen wird deshalb in diesem Temperaturbereich ausgeschlossen.
    Notes: The local structure in crystals, melts, supercooled melts, and glasses of sodium silicate hydrates of composition Na2O · SiO2 · nH2O (n = 9, 6, 5) is studied by variable temperature 1H, 23Na, and 29Si MAS NMR spectroscopy. Detailed in situ investigations on the melting process of the crystalline materials reveal the importance of H2O motion in the melting mechanism. Depending on the local coordination, crystallographically distinct Na sites show different behaviour during the melting process. Upon melting, the monomer silicate anions present in the crystalline hydrates undergo condensation reactions to oligomeric silicate anions. No recrystallization but glass formation occurs at low temperature if the melts were heated initially about 10 K above the melting point. In the glasses also oligomeric silicate anions are present with a preference for cyclotrimer species. In situ MAS NMR investigations and electric conductivity measurements of the melts, supercooled melts, and glasses suggest the distinction of three temperature ranges characterized by different local structure and dynamics of the sodium cations, water and silicate anions. These ranges comprise a glass and glass transition range A at low temperatures, an aggregation region B at intermediate temperatures, and a solution or electrolyte region C at high temperatures. In region B aggregation of sodium water complexes to hydrated polycation clusters is suggested, the dynamic behaviour of which is clearly different to that of the silicate anions, indicating that no long-lived contact ion pairs between sodium cations and silicate anions are formed.
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    Ein neuer Typ ternärer Cobaltsulfide A9Co2S7 (A \documentclass{article}\pagestyle{empty}\begin{document}$ \buildrel \wedge \over = $\end{document} K, Rb, Cs) mit trigonalplanaren [CoS3]-Baugruppen des zwei- und dreiwertigen CobaltsProfessor Peter Paetzold zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 405-408 
    Details
    ISSN: 0044-2313
    Keywords: Ternary cobalt sulphides ; preparation ; crystal structure ; magnetic properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Type of Ternary Cobalt Sulphide, A9Co2S7 (A \documentclass{article}\pagestyle{empty}\begin{document}$ \buildrel \wedge \over = $\end{document} K, Rb or Cs), containing Trigonal-Planar [CoS3] Units of Two- and Three-Valent CobaltThe passage of a stream of hydrogen over an alkali carbonate/cobalt/sulphur melt resulted in the preparation of the compounds K9Co2S7, Rb9Co2S7 and Cs9Co2S7. The structure of the potassium compound (Space group P213, Z = 4) could be determined from X-ray diffraction experiments on single crystals whilst X-ray investigations of powdered samples of the rubidium and caesium compounds indicate isotypic atomic arrangements with K9Co2S7. The characteristic structural elements of these compounds are trigonal-planar [CoS3]-units of two- and three-valent cobalt. The results from investigations of the magnetic properties of these ternary cobalt sulphides are in agreement with those expected for mixed-valent CoII/CoIII structures. The analogously-composed ferrates are closely structurally-related to these sulphides and show corresponding magnetic properties [1].
    Notes: Durch Schmelzreaktionen von Alkalicarbonat mit Cobalt und Schwefel im Wasserstoffstrom gelang die Darstellung der Verbindungen K9Co2S7, Rb9Co2S7 und Cs9Co2S7. Die Struktur der Kaliumverbindung konnte über röntgenographische Untersuchungen an Einkristallen bestimmt werden (Raumgruppe P213, Z = 4). Untersuchungen an pulverförmigen Proben lassen für die Rubidium- und die Cäsiumverbindung isotype Atomanordnungen erkennen. Als charakteristische Strukturelemente treten trigonal planare [CoS3]-Baugruppen des zwei- und dreiwertigen Cobalts auf. Untersuchungen zum Magnetismus sind in Übereinstimmung mit der Annahme eines gemischtvalenten Aufbaus, der auch bei den analog zusammengesetzten, in einem eng verwandten Strukturtyp kristallisierenden Ferraten auftritt [1].
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    Magnetische Wechselwirkungen in Inselstrukturen ternärer Cobaltchalkogenide. Die Spinstrukturen von Na6CoS4 und Na6CoSe4Professor Hans-Uwe Schuster in memoriam (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 412-416 
    Details
    ISSN: 0044-2313
    Keywords: Alkali transition metal chalcogenides ; magnetic structures ; neutron diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Magnetic Interactions in Ternary Cobalt Chalcogenides containing Isolated Tetrahedral Cobalt Anionic Groups. The Spin Structures of Na6CoS4 and Na6CoSe4The sodium cobalt chalcogenides Na6CoS4 and Na6CoSe4 are characterized by isolated [CoX4]-units. Despite the large distances of more than 6 Å between the cobalt ions magnetic inter-actions at low temperatures lead to threedimensionally ordered spin structures, that were determined from neutron diffraction experiments. The magnetic structure can be described in the Shubnicov group P2abc21 with a unit cell that is four times as large as the crystallographic cell. The magnetic moments of both compounds correspond to the value expected for three unpaired electrons per Co2+ ion.
    Notes: Die Natriumcobaltchalkogenide Na6CoS4 und Na6CoSe4 sind durch isolierte [CoX4]-Einheiten charakterisiert. Trotz der großen Abstände der magnetischen Zentren von über 6Å führen bei tiefen Temperaturen magnetische Wechselwirkungen zu dreidimensional geordneten Spinstrukturen, die über Neutronenbeugungsuntersuchungen aufgeklärt werden konnten. Die magnetische Struktur läßt sich in der Shubnikov-Raumgruppe P2abc21 mit einer Elementarzelle beschreiben, die gegenüber der kristallographischen das vierfache Volumen besitzt. Die Größe der magnetischen Momente entspricht dem für Co2+ zu erwartenden Wert von drei ungepaarten Elektronen.
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    Beiträge zum thermischen Verhalten von Sulfaten. XV [1]. Zum chemischen Transport von Al2(SO4)3 mit SOCl2. Experimente und ModellrechnungenProfessor Hans-Uwe Schuster in memoriam (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 417-423 
    Details
    ISSN: 0044-2313
    Keywords: Aluminium(III)-sulfate ; Chemical Transport ; Thermodynamical Calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions on the Thermal Behaviour of Sulfates. XV. The Chemical Vapour Transport of Al2(SO4)3 with SOCl2. Experiments and CalculationsWell shaped crystals (cubical or rectangular parallelepiped respectively) of rhombohedral Al2(SO4)3 can be grown in the less hot zone of a closed silica ampoule by means of chemical (vapour) transport using SOCl2 as transport agent in endothermal transport reactions. The influence of the mean transport temperature as well as the concentration of the transport agent on the deposition rates was investigated. We also tried to describe this transport system on the basis of thermochemical calculations.
    Notes: Gut ausgebildete Kristalle (würfel- bzw. quaderförmig) von rhomboedrischem Al2(SO4)3 wurden mit SOCl2 als Transportmittel im Temperaturgradienten (z. B. 625→525°C) auf der weniger heißen Seite einer Quarzglasampulle abgeschieden. Der Einfluß der Temperatur sowie der Transportmittelkonzentration auf die Abscheidungsraten wurde untersucht. Eine Interpretation des beobachteten, auf endotherme Reaktionen zurückzuführenden Transportverhaltens wird mit Hilfe thermodynamischer Modellrechnungen gegeben.
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    URL: http://dx.doi.org/10.1002/zaac.19956210314
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    Zur Kenntnis der ionischen Ozonide P(CH3)4O3 und As(CH3)4O3 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 431-434 
    Details
    ISSN: 0044-2313
    Keywords: Ionic ozonides ; preparation ; P(CH3)4O3 ; As(CH3)4O3 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Knowledge of the New Ionic Ozonides P(CH3)4O3 and As(CH3)4O3P(CH3)4O3 and As(CH3)4O3 were prepared via ion exchange in liquid ammonia and characterized by X-ray-powder, IR, MS and DTA techniques. P(CH3)4O3 and As(CH3)4O3 are isotypic and have a wurtzite-like arrangement of ions with rotationally disordered O3-. (Powder data: P63mc; P(CH3)4O3: a = 687.8(2), c = 964.6(3) pm; As(CH3)4O3: a = 708.6(1), c = 991.0(3) pm). As(CH3)4O3 shows a displacive phase transition at -135°C. The low temperature phase is orthorhombic (a = 715.8(7), b = 1 209(1), c = 943.3(1) pm).
    Notes: P(CH3)4O3 und As(CH3)4O3 wurden mittels Ionenaustausch in fl. NH3 erstmals dargestellt und mit Röntgenpulvermethoden, IR-Spektroskopie, MS und DTA charakterisiert. P(CH3)4O3 und As(CH3)4O3 sind isotyp und bilden eine Ionenpackung im Wurtzit-Typ mit fehlgeordnetem O3-. (Röntgenpulverdaten: P63mc; P(CH3)4O3: a = 687,8(2), c = 964,6(3) pm; As(CH3)4O3: a = 708,6(1), c = 991,0(3) pm). As(CH3)4O3 zeigt bei - 135°C eine displazive Phasenumwandlung. Die Tieftemperaturphase hat orthorhombische Metrik (a = 715,8(7), b = 1 209(1), c = 943,3(1) pm).
    Additional Material: 2 Tab.
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    LiBaBS3 und LiBaB3S6: Zwei neue quaternäre Thioborate mit trigonal-planar koordiniertem BorProfessor Hans-Uwe Schuster in memoriam (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 424-430 
    Details
    ISSN: 0044-2313
    Keywords: Thioborates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: LiBaBS3 and LiBaB3S6: Two New Quaternary Thioborates with Trigonally Coordinated BoronLiBaBS3 (P21/c; a = 7.577(2) Å, b = 8.713(2) Å, c = 8.687(2) Å, β = 116.22(2)°; Z = 4) und LiBaB3S6 (Cc; a = 15.116(3) Å, b = 8.824(2) Å, c = 8.179(2) Å, β = 117.46(3)°; Z = 4) were prepared by reaction of stoichiometric amounts of the metal sulfides, boron, and sulfur at 750°C. The anionic part of the structure of the orthothioborate LiBaBS3 consists of isolated planar [BS3]3- anions. The crystal structure of the metathioborate LiBaB3S6 contains [B3S6]3- anions formed by six-membered B3S3 rings with three exocyclic sulfur atoms. The metal cations are situated between the anion units leading to a ninefold sulfur coordination of the barium atoms and to a fivefold (LiBaBS3) and fourfold (LiBaB3S6) coordination of the lithium atoms.
    Notes: LiBaBS3 (P21/c; a = 7,577(2) Å, b = 8,713(2) Å, c = 8,687(2) Å, β = 116,22(2)°; Z = 4) und LiBaB3S6 (Cc; a = 15,116(3) Å, b = 8,824(2) Å, c = 8,179(2) Å, β = 117,46(3)°; Z = 4) wurden durch Reaktion stöchiometrischer Mengen der Metallsulfide mit Bor und Schwefel bei 750°C dargestellt. Die Anionenteilstruktur des Orthothioborats LiBaBS3 besteht aus isolierten, planaren [BS3]3--Anionen. Die Kristallstruktur des Metathioborats LiBaB3S6 enthält [B3S6]3--Anionen aus B3S3-Sechsringen mit drei exocyclischen Schwefelatomen. Die Metallkationen befinden sich jeweils zwischen den Anioneneinheiten, wobei für Barium eine neunfache, für Lithium eine fünffache (LiBaBS3) bzw. vierfache (LiBaB3S6) Koordination durch Schwefel beobachtet wird.
    Additional Material: 6 Ill.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280401
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    Tripodal Amides Containing a Totally Silicon-Based Ligand Framework (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 329-334 
    Details
    ISSN: 0009-2940
    Keywords: Trisilylsilanes ; Tripodal ligands ; Amido complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A novel type of tripodal amido ligand with a totally siliconbased (trisilylsilane-derived) ligand framework has been synthesized and coordinated to tetravalent titanium and zirconium. The key compound in the ligand synthesis is the chlorosilane H3CSi{Si(CH3)2CI}3 (2) which upon condensation with a range of primary amines R-NH2 (R = aryl, alkyl) yields the amino-functionalized ligand precursors H3CSi{Si(CH3)2NHR}3 (3a-e). Their corresponding trilithium salts have been found to be the appropriate amide transfer reagents in the subsequent syntheses of the transition metal complexes. Single-crystal X-ray structure analyses of the trilithium triamide H3CSi{Si(CH3)2N(Li)tBu}3 (4a) and the Ti complex H3CSi{Si(CH3)2N(p-Tol)}3TiBr (5b) have established their respective adamantane- and [2.2.2]bicyclooctane-related cage structures.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280403
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    Dilithium Derivatives of Bis(tert-butyldimethylsilylamino)silanes as Building Units for Inorganic Ring Compounds (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 351-355 
    Details
    ISSN: 0009-2940
    Keywords: Bis(silylamino)silanes ; Lithium compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The bis[(tert-butyldimethylsilyl)amino]silanes 1-3 are converted into their lithium derivatives 4-7 with BuLi. Depending on the bulkiness of the substituents, the dilithium derivatives 4 and 5 crystallize in cis or trans conformation. Monolithiated 3 (6) forms a four-membered (SiFLiN) ring system, while its dilithium salt is characterized as a lithium silyldiamide (7), Although 4, 5, and 7 have different structures, they react with PF3 (8, 9), SiF4 (10, 11), and CMe3SiF3 (12) as diamides to give the corresponding four-membered ring systems 8-12. The crystal structures of 4 and 5 are reported.
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    URL: http://dx.doi.org/10.1002/cber.19951280406
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    Carbohydratocarbene Complexes of Manganese and RheniumDedicated to Prof. Hans H. Brintzinger on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 373-378 
    Details
    ISSN: 0009-2940
    Keywords: Carbene complexes ; Carbyne complexes ; Carbohydrates ; Diastereoselective addition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The cationic carbyne complexes [Cp(CO)2M≡CR]+ [BX4]- [M = Mn, X = F: R = Ph (1), Tol (2); M = Re, X = 3,5-C6H2(CF3)2: R = Ph (3)] add the anion of monodeprotonated protected mannofuranose (4a), glucofuranose (4b), and fructopyranose (4c) to the carbyne carbon atom to form the carbohydratocarbene complexes 5a-c, 6a, b, and 7a. With 5b, 5c, and 6b the addition proceeds with retention of configuration at the anomeric center. Due to inversion of configuration in the deprotonation step the complexes 5a, 6a, and 7a are obtained as β-glycosides. The carbene ligand is oxidatively cleaved from the metal by trimethylamine N-oxide or air. Cleavage of the C(carbene)—O bond with reformation of the cation of the carbyne complex 2 is achieved by reaction of 6a with BCl3. Photolysis of [Cp(CO)2Mn=C(Ph)OEt] in the presence of L affords the carbene complexes [Cp(CO)(L)Mn=C(Ph)OEt] [L = P(OMe)3 (11), P(Tol)3 (12)]. Ethoxide abstraction from 11 and 12 by BF3 gives the chiral cationic carbyne complexes [Cp(CO)(L)Mn=CPh]+[EF4]- (13, 14) which add 4a to form the corresponding mannofura-nosylcarbene complexes (15, 16). When 0.5 equivalents of 4a are employed in the reaction with 13, 14 the ratio of diastereomers is 3:2, both for 15 and 16. Complex 11 was characterized by an X-ray structural analysis.
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    Ionenpaarbildung und Cyclisierungsreaktionen an koordinierten Oxalamidinen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 405-412 
    Details
    ISSN: 0009-2940
    Keywords: Sodium oxalamidinates ; 2-Imidazolidinone ; Ionic molybdenum carbonyl complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ion Pairing and Cyclization on Coordinatively Bound OxalamidinesThe tetraphenyloxalamidine ligand of complex 8a reacts easily in the presence of bases with elementorganic dichlorides (R2MCl2) to form coordinated metalacycles. The cyclization with phosgene gives the (CO)4Mo-coordinated 1,3-diphenyl-4,5-bis(phenylimino)-2-imidazolidinones 10. In contrast to the reaction forming the piperazine derivative 2, the reaction of 8a with oxalyl chloride also proceeds to 10 by decarbonylation. The product of this cyclization, (CO)4Mo(OCTPOA) (10), and two possible intermediates, the dinuclear sodium salts Na2(THF)8[(CO)4Mo(HTPOA)]2 (11a) and Na(THF)4[(CO)4Mo(EtO2COCTTOA)]2 (15) have been characterized by X-ray analyses. 11a contains the coordinated oxalaminate anion. The structure of the ionic complex 15 shows the simultaneous attack at both sp3-hybridized nitrogen atoms and the selective formation of the five-membered 2-imidazolidinone heterocycle by coordination of the oxalamidine. Both sodium complexes 11a and 15 are dimeric and centrosymmetric ion pairs. Complex 11a contains two C≡O—Na—O≡C bridges while compound 15 has a central [Na2O2] four-membered ring consisting of sodium alcoholate bridges.
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    URL: http://dx.doi.org/10.1002/cber.19951280412
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    Chiral Ligands for Transition Metal Complexation (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 449-454 
    Details
    ISSN: 0009-2940
    Keywords: Chiral ligands ; Transition metal complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Novel chiral salen- or salphen-type ligands with stereogenic centres in the 1,3-dicarbonyl moiety 2 as well as in the amino bridge in 15-18 were synthesized from the enantiomerically pure Hajos-Wiechert ketone.
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    URL: http://dx.doi.org/10.1002/cber.19951280503
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    Structure and Conformation of Bis(trifluoromethylthio)methane, CH2(SCF3)2 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 461-464 
    Details
    ISSN: 0009-2940
    Keywords: Bis(trifluoromethylthio)methane ; Gas-phase structure ; Conformational properties ; Electron diffraction ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The geometric structure and conformational properties of bis(trifluoromethylthio)methane, CH2(SCF3)2' were determined by gas electron diffraction. The main conformer (70 ± 15%) possesses C2 symmetry with dihedral angles Φ(SCSC) = 79.1(10)°. The second conformer possesses C1 symmetry. The following skeletal geometric parameters (distances ra [pm] and angles 〈α[°] with 3-σ uncertainties) were obtained: C—S 183.6(3), S—CF3, 179.3(3), S—C—S 112.1(6), and C—S—C 98.2(10). The geometric structures and relative conformational stabilities were well reproduced by ab initio calculations at the HF/3-21G* level.
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    URL: http://dx.doi.org/10.1002/cber.19951280505
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    Silicon Compounds with Strong Intramolecular Steric Interactions. LVIIPart LVI: Ref.[1].. Oxidation and Cycloaddition Reactions of an Unsymmetrically Substituted DisileneDedicated to Professor Manfred Regitz on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 935-939 
    Details
    ISSN: 0009-2940
    Keywords: Disilenes ; Organosilicon compounds ; 1,2,3-Oxadisiliranes ; Dioxadisiletanes ; Cycloaddition reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of the unsymmetrically substituted disilene R2Si=SiR′2 (4; R = 2,4,6-Me3C6H2, R′ = 2,4,6-iPr3C6H2) with m-chloroperbenzoic acid (mCPBA) or oxygen furnished the correspondingly substituted 1,2,3-oxadisilirane 5 or 1,3,2,4-dioxadisiletane 6, respectively. The [2 + 2] and [2 + 4] Cycloaddition reactions of 4 with benzophenone and 3,5-di-tert-butyl-1,2-benzoquinone, respectively, proceeded with a high degree of regioselectivity to yield the 1,2,3-oxadisiletane 9 and the 2,3-dihydro-1,4,2,3-benzodioxadisiline 7. The latter product was isolated together with a small amount of an isomeric compound 8 in which the substituents at the silicon atoms are reversed. The molecular structures of the products 5, 6, and 7 were determined by X-ray crystallography.
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    A Molybdenum-Catalysed Electrocyclisation-Cycloaddition Sequence: Synthesis and Structure of a Pentacyclic Unsaturated Ketone (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 953-956 
    Details
    ISSN: 0009-2940
    Keywords: Molybdenum oxadiene complex ; Cycloaddition ; Catalysis ; Stereoselectivity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The pentacyclic unsaturated ketone 3 is obtained as the sole product by the reaction of pinocarvone (1) with cycloocta-triene in the presence of catalytic amounts of dicarbonyl-bis(η4-pinocarvone)molybdenum (2). Compound 3 formally resulting from a [4 + 2] cycloaddition reaction of bicy-clo[4.2.0]octa-2,4-diene with the alkene fragment of pinocarvone was characterised by means of spectroscopy (1H, 13CNMR, IR, MS) as well as by X-ray crystal structure analysis. A mechanism is proposed involving rigid molybdenum complexes as intermediates in order to explain the stereospecificity of the reaction.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281001
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    Compounds of Germanium and Tin, 16Part 15: Ref.[1]. A Tetraaryldistannene with a Long Tin - Tin Multiple Bond and Differing Environments at the Tin Atoms (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 983-985 
    Details
    ISSN: 0009-2940
    Keywords: Diarylstannylene ; Tetraaryldistannene ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Although tetrakis(2-tert-butyl-4,5,6-trimethylphenyl)distannene (9), the first tetraaryl-distannene to be reported on, is stable in the solid state, only the monomeric stannylene 8 can be detected in solution. An X-ray crystal structure analysis of 9 reveals a long tin-tin bond length of 291.0(1) pm and a trans-bent Sn2C4 framework with different fold angles of 21.4° and 64.4°.
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    Synthesis and Structures of Magnesium TetrahydridoaluminatesDedicated to Dr. R. Bauer, who first synthesized magnesium tetrahydridoaluminate, on the occasion of his 70th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 999-1006 
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    ISSN: 0009-2940
    Keywords: Magnesium tetrahydridoaluminate ; Magnesium halide tetrahydridoaluminate ; (Organyloxo)magnesium tetrahydridoaluminates ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The molecular structures of XMg(A1H4) · 4 THF (1a, 2, 3a) (X = A1H4, Cl, Br) have been determined by X-ray structural analysis. Each compound possesses a hexacoordinated Mg center and AlH4- groups bound to this center via a single hydride bridge bond. Attempts to prepare ROMg(AlH4) compounds were successful only for sterically demanding groups R (R = CMe3, CPh3, naph, mes, smes). The 2-naphthoxy derivative 7, a compound with the composition (naphO)Mg-(AlH4) · 2.5 THF, is a dimer with a central Mg2O2 ring. One of its two AlH4- groups is terminally bound to one Mg atom, the other bridges the two Mg centers. This structure indicates how AlH4- transfer may occur from ROMg(AlH4) compounds to form Mg(OR)2 and Mg(AlH4)2.
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    Functionalized Diorganozinc Compounds: Key Reagents for the Synthesis of Enantiomerically Pure 2,5-Disubstituted cis- and trans-Tetrahydrofurans (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1021-1028 
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    ISSN: 0009-2940
    Keywords: Synthesis, stereoselective ; Catalysis ; Tetrahydrofurans ; Dialkylzinc reagents ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,4-Diol derivatives 4a-i were synthesized stereoselectively by either reagent- or catalyst-controlled routes using the addition of functionalized diorganozinc reagents to aldehydes. The stereoselectivities along the reagent-controlled synthetic path were in the range between 80:20 and 95:5. The stereoselectivities along the catalyst route exceeded 95:5. The 1,4-diol derivatives 4 thus obtained were transformed into enantiomerically pure cis- and trans-2,5-disubstituted tetrahydrofurans (16-20) by means of an intramolecular Williamson reaction.
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    Amino Substituted Tricarbonyl(cyclobutadiene)iron Complexes: Pd-Catalyzed Coupling of Iodocyclobutadiene Complexes with Amines (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1055-1058 
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    ISSN: 0009-2940
    Keywords: Aminations ; Palladium catalysis ; Organometallic amines ; Coupling reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The coupling of the iodides 1 with amines under palladium catalysis affords the novel aminated cyclobutadiene derivatives 2 in preparative useful yields.
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    URL: http://dx.doi.org/10.1002/cber.19951281016
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    Addition von Hydrofullerid [C60H]- an koordinierte, ungesättigte Kohlenwasserstoffe: Bindung von Fulleren an Metallkomplexe über KohlenwasserstoffbrückenHerrn Professor Herbert Walter Roesky zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1059-1060 
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    ISSN: 0009-2940
    Keywords: Fullerene ; Hydrofulleride ; Manganese complex ; Rhenium complex ; Iron complexes ; Ruthenium complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Addition of Hydrofulleride [C60H]- to Coordinated, Unsaturated Hydrocarbons: Binding of Fullerene to Metal Complexes through Hydrocarbon BridgesHerrn Professor Herbert Walter Roesky zum 60. Geburtstag gewidmet.Hydrofulleride [C60H]- is added to the hydrocarbon ligands of the cationic complexes [(OC)5Re(η2-C2H4)]+, [(OC)3Mn-(η6-C6H6)]+, [(OC)3M(η5-C6H7)]+ (M = Fe, Ru), [(OC)3Fe(η5-C7H9)]+, and [(η5-C5H5)Fe(η6-C5H4CH2)]+.
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    Metal Complexes of Functional Isocyanides, XXV. Amino(hydrazino)carbene Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1061-1068 
    Details
    ISSN: 0009-2940
    Keywords: N-Isocyanides ; N-Isocyanodialkylamine complexes ; Carbene complexes ; Imaging-Plate data collection ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The N-isocyanodialkylamine metal complexes [M(CO)5CN-NR2] (M = Cr, W), trans-[MI2(CNNR2)2] (M = Pd, Pt), trans-[Pt(Cl)(CNNR2)(PPh3)2]BF4, and cis-[PtCl2(CNNR2)(PPh3)] [R = Et, iPr; 2 R = -{CHMe(CH2)3CHMe}-] react with primary amines to give the amino(hydrazino)carbene metal complexes [M(CO)5(C(NHR′)NHNR2}] (R′ = Me, nPr, Cy) (1-9), trans-[PtI2{C(NHMe)NHNR2}2] (10-12) and trans, and the amine adducts cis-[PtCl2{C(NHMe)NHNC(H)(Me) (CH2)3CHMe}(PPh3)] H2NMe (14), and trans-[PdI2{C (NHMe)NHNC(H)(Me)(CH2)3CHMe}2] 2 H2NMe (15). With secondary amines the amino(hydrazino)carbene metal complexes trans (18) and trans-[PtCl{C(NEt2)NHNEt2} (PPh3)2]BF4 (19) Were isolated. The complexes trans-[PtI2{C(NHCy)NHNiPr2}CNNiPr 2] (20) and trans-[PdI2 (NH2Cy){C(NHCy)NHNiPr2}] (21) were obtained by reaction of trans-[MI2(CNNiPr2)2] (M = Pd, Pt) with cyclohexylamine. The structures were assigned on the basis of IR, NMR- (1H, 13C, 31P), and mass spectroscopy as well as an X-ray structural analysis of 21.
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    Thiaaza-arachno-pentaboran SNB3H2tBu3R (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1105-1108 
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    ISSN: 0009-2940
    Keywords: Azadiboriridine, tri-tert-butyl- ; Mercaptoborane ; Thiaaza-arachno-pentaborane, 1,4,5-tri-tert-butyl-2-organo- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thiaaza-arachno-pentaborane SNB3H2tBu3RThe azadiboriridine [-B(tBu)-N(tBu)-B(tBu)-] (1) gives 1:1 adducts with the mercaptoboranes BH2(SR), which can be generated from their cyclotrimers by the action of THF. The adduct 4a (R = Ph), a nido cluster with an NB3 skeleton, forms an equilibrium with an adduct 5a, an arachno cluster with an SNB3 skeleton, whose S-bound ligand Ph is found in an endo position by an X-ray structural analysis. The equilibrium 4a · 5a involves a Lewis acid-base reaction, which is electronically coupled to a reduction of a three-center to give a two-center π bond. The reaction of 1 with BH2(SPr) gives the corresponding arachno cluster 5b only.
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    Metallkomplexe mit biologisch wichtigen Lisganden, LXXXLXXIX. Mitteilung: Lit.. (η3:η3-C10H16)Ru(IV)-Komplexe mit α-Aminocarboxylaten, α-Aminosäureestern und Peptidestern als Liganden (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1117-1125 
    Details
    ISSN: 0009-2940
    Keywords: 1,7-Dimethylocta-2,6-diene-1,8-diyl ; Ruthenium complexes ; α-Amino carboxylates ; α-Amino acid esters ; Peptide esters ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Complexes Containing Biologically Important Ligands, LXXXLXXIX. Mitteilung: Lit. .  -  (η3:η3-C10H16)Ru(IV) Complexes with α-Amino Carboxylates, α-Amino Acid Esters, and Peptide Esters as LigandsReactions of the chloro-bridged bis(allyl) complex [(η3:η3-C10H16)Ru(Cl)(μ-Cl)]2 with α-amino carboxylates and α-amino acid esters afford the complexes (η3:η3-C10H16)(Cl)RuNH2CHRCO2 (2) and (η3:η3-C10H16)(Cl)2-RuNH2CHRCO2R′ (3). Abstraction of chloride from 3 by Ag+ gives the N,O-chelates [(η3:η3-C10H16)(Cl)RuNH2CHRCO2R′]+BF4 (4). Cysteine methyl ester forms the N,S-chelate complex (η3:η3-C10H16)(Cl)RuNH2CH(CO2CH3)CH2S (5), and with histidine methyl ester a dinuclear complex 6 with N,N-histidine bridge is obtained. Compound 3d with L-PheOEt as ligand was characterized by X-ray diffraction.
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    Erste strukturelle Charakterisierung eines 3-Silaoxetans und 3-Silathietans im Kristall und in Lösung (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 167-172 
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    ISSN: 0009-2940
    Keywords: 1-Oxa-3-silacyclobutane ; 1-Thia-3-silacyclobutane ; 3-Silaoxetane ; 3-Silathietane ; Solid-state NMR, 13C, 29Si ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: First Structural Characterisation of a 3-Silaoxetane and a 3-Silathietane in the Crystal and in SolutionThe 3-silaoxetane 3,3-dimethyl-2,2,4,4-tetraphenyl-1-oxa-3-silacyclobutane (1) and the 3-silathietane 3,3-dimethyl-2,2,4,4-tetraphenyl-1-sila-3-thiacyclobutane (2) were synthesized and studied in the solid state and in solution. The crystal structures of 1 and 2 were investigated by X-ray diffraction. Furthermore, 1 and 2 were characterized by solid-state NMR spectroscopy (13C and 29Si CP/MAS). The cyclobutane ring of 1 is planar with a C-Si-C angle of 75.07(9)° and a C-O-C angle of 105.3(2)°. 2 crystallizes with a non-planar cyclobutane ring with a C-Si-C angle of 89.00(11)° and a C-S-C angle of 93.25(11)°. The Si-O distance of 241.5(3) pm for 1 and the Si-S distance of 263.9(3) pm for 2 are shorter than the sum of the van der Waals radii of these atoms. The results obtained by X-ray diffraction are consistent with those from solid state 13C-NMR spectroscopy for 1 and 2. Different 29Si-NMR spectra in solution and the solid state indicate unusual electronic or steric effects around the silicon atom of 2 in the solid.
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    Zwei Extreme in der Zinnchemie: Ein nichtbindender Sn-Sn-Abstand von 285 pm und eine 119Sn-NMR-Verschiebung δ = 3301 in metallorganischen Derivaten von Sn(0)Herrn Prof. Dr. G. P. Schiemenz gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 187-191 
    Details
    ISSN: 0009-2940
    Keywords: Tin complexes ; Transition metal complexes ; NMR, 119Sn ; Sn(0) compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two Extremes in Tin Chemistry: A Non-bonding Sn-Sn Distance of 285 pm and a 119Sn-NMR Shift δ = 3301 in Organome-tallic Derivatives of Sn(0)The reaction of Na[{Cp'(CO)2Mn}2H] with SnCl2, which produces the inidene compound [Cp'(CO)2Mn\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ {\rm C}\ddot - {\rm C} $\end{document}Sn(Cl)\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ {\rm C}\ddot - {\rm C} $\end{document}Mn-(CO)2Cp']- under standard workup procedures, results in the formation of [{Cp'(CO)2MnSn}2{μ2-Mn(CO)2Cp'}2{μ2-Cl}]- (1) when quenched with unpolar solvents. While, formally, 1 contains tin in its oxidation state zero, it may be conceived as composed of an Sn2-2 entity, which is linearly end-on coordinated to two Cp'(CO)2Mn 16-electron species; in addition the tin centers are bridged by two μ2-Mn(CO)2Cp' moieties and a μ2-Cl function. The resulting connectivity Sn2{μ2-Mn(CO)2Cp'}2{μ2-Cl} thus corresponds to a [1.1.1]propellane scaffolding. While there is no obvious need for a tin-tin bond in this propellane-type cage, a short Sn-Sn contact of only 285 pm is observed. While the 119Sn-NMR signal of 1 could not be recorded, the peculiar bonding in this type of compounds is generally mirrored in their unconventional 119Sn-NMR shift whereever signals can be observed: it is found that [{Cp*(CO)2Mn}3(μ3-Sn)], which contains trigonally planar-coordinated μ3-Sn as a naked ligand atom, has its 119Sn-NMR resonance at δ = 3301 well beyond the known range of 119Sn-NMR shifts. This finding is interpreted in terms of a relatively week Snpπ-Mndπ π bonding which leads to low-energy unoccupied molecular orbitals as the prerequisit for a large paramagnetic contribution to the NMR shift.
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    Darstellung und Charakterisierung der Tetrahedrane [CpM(CO)2]3P (M = Mo, W) sowie der Derivate [CpMo(CO)2]3P-Mo(CO)5 und [CpW(CO)2]3P-W(CO)5 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 197-199 
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    ISSN: 0009-2940
    Keywords: μ3-Phosphorus-trimolybdenum tetrahedrane ; μ3-Phosphorus-tritungsten tetrahedrane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Characterization of the Tetrahedranes [CpM(CO)2]3P (M = Mo, W) and Their Derivatives [CpMo(CO)2]3P-Mo(CO)5 and [CpW(CO)2]3P-W(CO)5The reaction of Na[CpM(CO)3] (M = Mo, W) with PCl3 in diglyme yields the cluster compounds [CpMo(CO)2]3P-Mo(CO)5 (2a) and [CpW(CO)2]3P-W(CO)5 (2b) in good yields as well as the tetrahedranes [CpMo(CO)2]3P (3a) and [CpW(CO)2]3P (3b) as side products. Compounds 3a, b are obtained independently by the reaction of 2a, b with PPh3. The clusters 2a, b and 3a, b were characterized spectroscopically (IR, NMR, MS), and X-ray structure determinations were carried out on 2a, b.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/cber.19951280301
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    Contributions to the Chemistry of Boron, 227Part 226: Ref.. The P-centered Chemistry of [(Di-tert-butylphosphanyl)imino]-(2,2,6,6-tetramethylpiperidino)boraneDedicated to Professor Helmut Werner on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 205-212 
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    ISSN: 0009-2940
    Keywords: Borane, [(di-tert-butylphosphanyl)imino](2,2,6,6-tetramethylpiperidino) dimer ; Phosphonium, di-tert-butylmethyl[(2,2,6,6-tetramethylpiperidinoborylene)imino]iodide ; Haloboration ; Hydroboration ; Metal carbonyl complexes of [(di-tert-butylphosphanyl)imino](2,2,6,6-tetramethylpiperidino)borane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The elements oxygen, sulfur, and selenium add to the P atom of the title borane 1. In contrast to the formation of tmp—B≡N—P(X)tBu2 (X = S, Se), the P oxide (X = O) dimerizes to [tmp—B≡N—P(O)tBu2]2 (5) with an eight-membered flat boat-shaped B2N2P2O2 ring. Borane 1 reacts readily with Mel to yield a phosphonium salt 8 and with BBr3 to give an adduct 9 with a B—P bond. In contrast, bis(dichloroboryl)-methane not only adds to 1 to generate a coordinate B—P bond but also chloroborates the B≡N triple bond, the final product being a new five-membered heterocycle 10. Similarly, the BH3 component of BH3·SMe2 first adds to the P atom of 1 followed by reaction of a second mol of BH3·SMe2 which hydroborates the B≡N triple bond. Finally, metal carbonyl fragments add only to the P atom of 1, demonstrating also that the chemistry of the molecule 1 is dominated by the basicity of its P center.
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    Photocatalytic Oxygenation of Selected Cycloalkenes in Aqueous Solutions Induced by Water-Soluble Metal Porphyrin Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 229-234 
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    ISSN: 0009-2940
    Keywords: Photooxygenation ; Dioxygen activation ; Metalloporphyrins ; Epoxidation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Water-soluble manganese(III) as well as iron(III) porphyrinates are introduced as light-sensitive precursor compounds for the photocatalytic activation of dioxygen in aqueous solutions. It is shown that in the presence of α-pinene (4) and the further cycloalkenes 11-13 photocatalytic oxygenation reactions occur. The dependence of the selectivity of the oxygen transfer to the olefin on both the presence of water and the variation of the substrate-to-catalyst ratio is discussed. The catalyst may be conveniently separated from the substrates/products by using aqueous solvent systems.
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    Ylidyl-dihalogenphosphane - Strukturbilder einer sich anbahnenden Dissoziation (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 379-393 
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    ISSN: 0009-2940
    Keywords: Ylides, dichloro- and dibromophosphanyl- ; Enamines, dichlorophosphanyl- ; Phosphonium ions, chlorophosphaalkenyl- ; Stereoelectronic (anomeric) effect and anionic hyperconjugation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ylidyl-dihalophosphanes Provide Structural Snapshots on Their Way to DissociationThe reaction of phosphonium ylides with phosphorus trihalides has been studied for the synthesis of ylidyl-dihalophos-phanes (= dihalophosphanyl ylides) Ph3P=CR—PX2 3, X = Cl, and 9, X = Br. Compounds 3, R = aryl, are readily prepared from the phosphonium bromides [Ph3P—CH2R]Br, compounds 3, R = alkyl, SiMe3 or PCl2, and 9 are obtained from silylylides Ph3P=CR—SiMe3, compound 3, R = PPh3+ results from the addition of PCl3 to the hexaphenylcarbodiphosphorane. A (β-morpholinovinyl)dichlorophosphane 12 has also been prepared. Ylides 3 are oxidized by sulfur and selenium and are converted to ylidyl-chlorophosphenium (= chloro-phosphaalkenyl-phosphonium) salts [Ph3P—CR=PCl]AlCl4 10. In the 31P-NMR spectra of 3 and 9 the geminal coupling 2JPP indicates the phosphorus lone pair to be synperiplanar to the phosphonio group. In one case the P(III)—C rotation barrier has been estimated from VT-31P-NMR spectra. By X-ray crystallography the structures of 3, R = Me, 2,6-Cl2C6H4, 4-NO2C6H5, PCl2, of 9, R = Me (two molecules), SiMe3, of an ylidyl-selenophosphonyl dichloride (11b), and of 12 have been analyzed. They provide representatives for the full range of rotation from the symmetric conformer with two equal P—X bonds to the conformer with one P—X bond perpendicular to the PCP plane and with this bond being extremely elongated. Thus, they map out the pathway to P—X bond breaking. On this way the initial charge transfer from the ylidic carbon to the antibonding P—X orbital ends up in a π donation and P—X dissociation.
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    Mono- und Diferriophosphane und -thioxophosphoraneHerrn Professor Dr. Ekkehard Lindner zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 413-416 
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    ISSN: 0009-2940
    Keywords: Ferriophosphanes ; Ferriophosphoranes ; Thioxophosphane ligand ; Decarbonylation reaction ; Sulfurization ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mono- and Diferriophosphanes and -thioxophosphoranesHerrn Professor Dr. Ekkehard Lindner zum 60. Geburtstag gewidmet.The substitution of organic substituents in phosphanes or thioxophosphoranes by the 17-electron fragments CpFe-(CO)2 (—Fp) leads to isolobal ferriophosphanes or -thioxophosphoranes. The mono- and diferriophosphanes FpnPPh3-n [n = 1 (3), 2 (4)] are obtained by deprotonation of the mono- and diferriophosphonium salts [FpnPPh3-nH]X [n = 1 (1), 2 (2)] with DBU. They are oxidized by sulfur giving the mono- and diferriothioxophosphoranes FpnPPh3-n(S) [n = 1 (5), 2 (6)]. Sulfide 5 arises also from the reaction of CpFe(CO)2Cl and Ph2PH(S)/DBU. The one-sided decarbonylation reaction of 6 leads to FpFp′PPh(S) (7, Fp′ = CpFeCO). The Fp substituents (17 electrons) in 3-7 coordinate as one-electron donors to the PhnP- or PhnP(S) units (n = 1, 2). The bridging functions in 4 and 6 are hitherto unknown. The molecular structures of the complexes 5-7 were determined by X-ray structure analyses.
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    Metallorganische Verbindungen der Lanthanoide, 89. Cyclooctatetraenyl-Komplexe der frühen Übergangsmetalle und Lanthanoide, 6. (Cyclooctatetraenyl)[N,N′-bis(trimethylsilyl)benzamidinato]-und -[diphenylbis(trimethylsilylimido)phosphinato]-Komplexe der Seltenen Erden; Röntgenstrukturanalyse von (C8H8)Tm[PhC(NSiMe3)2](THF), (C8H8)Lu[4-MeOC6H4C(NSiMe3)2](THF) und (C8H8)Nd[Ph2P(NSiMe3)2](THF) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 395-404 
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    ISSN: 0009-2940
    Keywords: Lanthanides, organo-, complexes ; Cyclooctatetraenyl complexes ; Benzamidinate ligands ; Diimidophosphinate ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organometallic Compounds of the Lanthanoids, 89. - Cyclooctatetraenyl Complexes of the Early Transition Metals and Lanthanoids, 6. - (Cyclooctatetraenyl)[N,N′-bis(trimethylsilyl)benzamidinato]- and -[diphenylbis(trimethylsilylimido)-phosphinato] Complexes of the Rare Earths; X-Ray Structural Analyses of (C8H8)Tm[PhC(NSiMe3)2](THF), (C8H8)Lu[4-MeOC6H4C(NSiMe3)2](THF), and (C8H8)Nd[Ph2P(NSiMe3)2](THF)[(C8H8)Ln(μ-Cl)(THF)2]2 or [(C8H8)Ln(μ-O3SCF3)(THF)2]2 (Ln = Y, Ce, Pr, Nd, Sm, Tm, Lu) react with Na[4-RC6H4C(NSiMe3)2] (R = H, OMe, CF3) or Li[PhC(NSiMe3)2] to give the monomeric (cyclooctatetraenyl)lanthanide benzamidinates (C8H8)Ln[4-RC6H4C(NSiMe3)2](THF) [R = H, Ln = Y (1), Ce (4), Pr (6), Nd (8), Sm (10), Tm (12), Lu (15); R = OMe, Ln = Y (2), Ce (5), Pr (7), Nd (9), Sm (11), Tm (13), Lu (16); R = CF3, Ln = Y (3), Tm (14), Lu (17)]. The reaction of [(C8H8)Ln(μ-Cl)(THF)2]2 (Ln = Ce, Pr, Nd, Sm) with Li[Ph2P(NSiMe3)2] in THF leads directly to the monomeric compounds (C8H8)Ln[Ph2P(NSiMe3)2](THF) [Ln = Ce (18), Pr (19), Nd (20), Sm (21)] in good yields. The 1H-, 13C-, 31P- and 29Si-NMR and mass spectra of the new compounds as well as the molecular structures of 12, 16, and 20 are discussed. The Raman spectra of the complexes 1-3, 12, and 14-17 have been studied in detail.
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    Syntheses of Cyclic and Acyclic Bis(perfluoroalkylthio)nitronium Salts (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 429-433 
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    ISSN: 0009-2940
    Keywords: Nitronium ions ; One-electron oxidation ; Superacidic systems ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (F3CS)3N (1) is oxidized quantitatively by AsF5 to the first bis(perfluoroalkylthio)nitronium salt (F3CS)2N+AsF-6 (2). Addition of halide ions (F-, Cl-, Br-, l-) to the cation of 2 destroys the S—N—S chain. (F2CSCl)2 undergoes with ammonia a cyclization reaction to S—CF2—CF2—S—N—H (3), which can be derivatized with F3CSCl or (F2CSCl)2 to S—CF2—CF2—S—N—SCF3 (3a) and (S—CF2—CF2—S—N—SCF2—)2 (3b), respectively. Oxidation of 3a with AsF5 yields (S—CF2—CF2—S—N+AsF-6 (4) and byproducts, which suggest formation of a {3a}+• radical cation as an intermediate in this reaction. Pure 4 is accessible by reaction of 3 with AsF5 in 54% yield. The chemical and spectroscopic properties of the new species are discussed.
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    Syntheses and Properties of X6Te2N2Se (X=Cl, Br): Stable Heterocycles with an N=Se=N Moiety (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 437-439 
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    ISSN: 0009-2940
    Keywords: Ditellurium(IV), di-μ-halogeno-tetrahalogeno-μ-(selenium diimidato) ; Selane, bis[bis(trimethylsilyl)amido]- ; Diselane, bis[bis(trimethylsilyl)amido] ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of Se[N(SiMe3)2]2 with TeX4 (X=Cl, Br) yields new bicyclic tellura heterocycles X6Te2N2Se (X=Cl, 1a; X=Br, 1b). Similarly, these compounds are obtained with elimination of elemental selenium by reaction of Se2-[N(SiMe3)2]2 with TeX4 (X=Cl, Br). They are characterized by IR and mass spectroscopy as well as elemental analyses. 125Te- and 77Se-NMR data are given for Cl6Te2N2Se (1a), and spectra are compared with those of the corresponding sulfur analogs.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280501
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    Synthesis and Structure of the First Dimetalated Diphosphane Disulfide [(η5-C5Me5)(CO)2FeP(H)(S)]2 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 441-442 
    Details
    ISSN: 0009-2940
    Keywords: Diphosphane disulfides ; Metallophosphoranes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The first transition metal derivative meso-[(η5-C5Me5)(CO)2FeP(H)(S)]2 (2) of the unknown diphosphane disulfide [PH2(S)]2 results from treatment of (η5-C5Me5)(CO)2FePH2 (1) with 1.5 equivalents of elemental sulfur. Compound 2 was characterized by means of spectroscopy (IR, 31P, 31P{1H}, 13C{1H}, 1H NMR) as well as X-ray diffraction analysis.
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    URL: http://dx.doi.org/10.1002/cber.19951280419
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    Molecular Modeling, a Tool for Predicting Structural Effects on the Macrocyclization Reaction between Bis(vinyl or allyl) Dialdehydes and Thiophosphonic Bis(hydrazides) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 443-447 
    Details
    ISSN: 0009-2940
    Keywords: Phosphorus macrocycles ; Molecular modeling ; Cyclocondensation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of new phosphorus dialdehydes PhP(O)-[(CH2)nCH=CHC6H4CHO]2 (4a-c, 5a) (n = 0:4, n = 1:5; a:para, b:meta, c:ortho), with thiophosphonic bis(hydrazide) PhP(S)[NMeNH2]2 (6) yields macrocyclic compounds 9b′, c′, 10a′, 9a″, b″, c″, 10a″ and 9c′″, arising from the cyclocondensation of one, two, or three equivalents of each reagent, respectively. Molecular modeling of 4a-c, 5a, 6 and of the intermediate monocondensation products 7a-c, 8a was carried out and points out the importance of the geometry of the starting reagents in the competition between inter- and intramolecular cyclocodensation.
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    URL: http://dx.doi.org/10.1002/cber.19951280502
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    Novel Aromatic Azopolymers with Regularly Interposed Tellurium Atoms in the Backbone (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 703-709 
    Details
    ISSN: 0009-2940
    Keywords: Copolymers ; Electrical conductivity ; Azo compounds ; Tellurides, organo ; Telluration ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Previously unknown alt-copoly(telluro-1,4-phenylene/azo-1,4-phenylene) and related polymers were synthesized by several different approaches, which include a) reductive polymerization of bis(4-nitrophenyl) tellurides with zinc; b) oxidative polymerization of bis(4-aminophenyl) telluride using a CuI/CuII redox system as catalyst under oxygen; c) electrochemical polymerization of bis(4-amino-3,5-dimethylphenyl) telluride; d) condensation polymerization of 1,4-dinitrosobenzene with bis(4-aminophenyl) telluride Te, Te-dichloride, and e) condensation polymerization of bis(4-nitrophenyl) telluride with bis(4-aminophenyl) telluride in the presence of sodium hydroxide. The polymers obtained were characterized by elemental analysis, 13C-CPMAS NMR, IR and UV-vis spectroscopy, GPC, and inherent viscosity measurements, and their properties were examined, particularly their electrical conductivity. The electrical conductivities of the new polymers 9b c, and 10 were shown to increase from below 10-7 up to 10-5 ∽ 10-2 S cm-1 upon bromine doping in spite of their formally interrupted conjugation structure.
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    URL: http://dx.doi.org/10.1002/cber.19951280708
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    Synthesis of Allenes by 1,6-Addition of Organocuprates to Acceptor-Substituted Enynes: Scope and Limitations (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 851-860 
    Details
    ISSN: 0009-2940
    Keywords: Allenes ; 1,6-Addition ; Cuprates, organo- ; Allenyl enolates ; Electrophiles, regioselective reaction of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Acyclic acceptor-substituted conjugated enynes bearing sulfonyl sulfinyl, sulfonate, nitro, amide, cyano, and oxazolidino groups at the double bond were synthesized and the regioselectivity of their reaction with organocuprates was examined. All Michael acceptors except enynes with nitro and amide functions underwent 1,6-additions, and the allenyl enolates thus formed were trapped with electrophiles in order to obtain the corresponding allenes. A qualitative reactivity scale for these reactions was established. The dependence of the regioselectivity of both the cuprate addition and the subsequent electrophilic capture on the acceptor group and the substitution pattern of the allenyl enolate were studied. Cyclic 2-en-4-ynoates with endocyclic double bonds were synthesized and treated with organocuprates to afford an exocyclic allene in one case.
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    URL: http://dx.doi.org/10.1002/cber.19951280902
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    Synthesis of 7-Alkyl/aryl-1,3,5-triaza-7-phosphonia-adamantane Cations and Their Reductive Cleavage to Novel N-Methyl-P-alkyl/aryl[3.3.1]bicyclononane Ligands (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 891-900 
    Details
    ISSN: 0009-2940
    Keywords: 1,3,5-Triaza-7-phospha-adamantane ; Reductive cleavage of phosphonium salts ; Ambidentate P,N-ligands ; P,N-[3.3.1]bicyclononane systems ; Phosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two reaction pathways for the synthesis of 1,3,5-triaza-7-phosphoniaadamantane salts, RP[(CH2)6N3]+X- (1), were followed. Route 1 starts with commercial tetrakis(hydroxymethyl)phosphonium chloride, which is converted into P(CH2OH)3 by treatment with a base. Subsequent quaternization with alkyl halides RX and cyclization with formaldehyde and ammonia afford [R-TPA]+X-. This process is only applicable for R = Me (1a) and Et (1b), however. Route 2 is more general and starts with primary phosphanes RPH2, which are converted into organotris(hydroxymethyl)phosphonium salts with formaldehyde and hydrochloric acid followed by ring closure with CH2O/NH3 to give compounds 1c-1f (R = t-Bu, c-Hex, Bz, and Ph, respectively, and X = Cl, I, PF6, or BPh4). Reductive cleavage of compounds 1 by sodium in liquid ammonia proceeds with either external (P-R) or internal (P-CH2) bond rupture. P-R cleavage affords the 1,3,5-triaza-7-phosphaadamantane (TPA), while cage cleavage leads to new bowl- or helmet-shaped ligand systems with peripheral amine and phosphane functions (2). Yields of the cage-opening reaction are highest for R = Ph (2f), moderate for R = Me and Et (2a, 2b), and poor with the remaining R groups (2c-2e). A radical mechanism is proposed for this reaction, the leaving group properties of R determining the direction of the cleavage. The crystal and molecular structures of compounds 2a and 2f were determined by X-ray diffraction studies. Exo positions were found for the N-Me and P-R groups. The isomers with the R group in the endo position are also present in solution in small amounts, as detected by NMR spectroscopy. Isomer interconversion by P inversion is slow on the NMR time scale. Compounds 2a, 2b and 2f were oxidized with elemental sulfur and selenium to give the monosulfides and selenides, respectively (2aS, 2aSe, 2bS, 2bSe, 2fS, 2fSe). Oxidation with H2O2 led to degradation. Compound 2a was quaternized at the P atom by treatment with Mel to give the corresponding phosphonium salt. Treatment with equimolar quantities of (Me2S)AuCl led to the 1:1 complexes 2aAucl, 2bAuCl and 2fAuCl, with the AuCl units solely P-bonded, as determined by X-ray diffraction of 2aAuCl and 2fAuCl. Compound 2a forms an ionic 2:1 complex with AuCl, composed of the ions [(2a)2Au]+ Cl- (with unidentate ligands), while its reaction with [Me2AuCl]2 leads to [Me2Au(2a)]+ [Me2AuCl2]- (with a chelating 2a ligand), as again confirmed by crystal structure analysis in both cases. Ligands 2a, 2b and 2f also act as chelating ligands in their tetracarbonylmolybdenum complexes obtained in the reactions with (C7H8)Mo(CO)4.
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    Controlled Conversion of the Transient 2-Mesityl-1,1-bis(trimethylsilyl)silene into a Tetrahydro-2,3-disilanaphthalene, a 1,2-Disilacyclobutane, or a 1,3-Disilacyclobutane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1083-1088 
    Details
    ISSN: 0009-2940
    Keywords: Silenes ; Silene dimerization ; 1,2-Disilacyclobutanes ; 1,3-Disilacyclobutanes ; 2,3-Disilanaphthalene, tetrahydro- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mesityl[tris(trimethylsilyl)silyl]methanol (1) reacts with strong bases with elimination of trimethylsilanolate according to a Peterson-type mechanism, the outcome of the reaction being dependent on solvent, temperature, and nature of the organometallic base applied. Thus, 1 was converted by treatment with MeLi in ether at -78°C to (E)-1,2,3,8a-tetra -hydro-1-mesityl-5,7,8a-trimethyl-2,2,3,3-tetrakis (trimethylsi-lyl)-2,3-disilanaphthalene (3), formally a [2 + 4] cyclodimer of the transient silene (Me3Si)2Si=CHMes (2). The reaction of 1 with PhMgBr in THF after some days resulted in the formation of (Z)-3,4-dimesityl-1,1,2,2-tetrakis(trimethylsilyl) -1,2-disilacyclobutane (6) as the main product besides small quantities of 3, the polysilane (Me3SiSi(SiMe3)2CH2Mes (10), and the alkoxysilane (Me3Si)3SiCH(Mes)OSi(Si-Me3)2CH2Mes (7). Compound 6, the formal [2 + 2] cycloadduct of 2, can also be obtained by thermal treatment of 3 and is considered to be the thermodynamically more stable silene dimer whereas 3 is the kinetically preferred product. At high LiBr concentrations in the reaction mixture 1 was converted by PhMgBr in THF to (E)-2,4-dimesityl-1,1,3,3-tetrakis(tri- methylsilyl)-1,3-disilacyclobutane (13) besides 6 and [bis(tri-methylsilyl)silyl]mesityl(trimethylsiloxy)methane (11). The unforeseen formation of 13 is discussed as proceeding via the silene-lithium bromide adduct (Me3Si)2Si(Br)CH(Li)Mes (12). In the absence of LiBr 1 was converted by MeLi in THF at -78°C to 11 and the trisilane (Me3Si)2Si(Me)CH2Mes (4b). Probable pathways of the formation of all new compounds are discussed. For 6 and 13 the results of the X-ray structural analyses are given.
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    URL: http://dx.doi.org/10.1002/cber.19951281105
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    Highly Substituted Tris(pyrazolyl)methane Ligands and Some Zinc Complexes Thereof (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1095-1103 
    Details
    ISSN: 0009-2940
    Keywords: Zinc complexes ; Tridentate ligands ; Tris(pyrazolyl)methane ; Reactivity ; Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(pyrazolyl)methane ligands in which two or three of the pyrazole carbon atoms bear organic substituents (L1-L7) were synthesized from chloroform and the corresponding pyrazole under phase transfer conditions. Their behavior towards zinc salts was found to span the range from no reaction at all to hydrolytic destruction. One hydrolysis product isolated and structurally characterized was the perchlorate complex [(HPz5)3Zn-OClO3]ClO4 (1), other ones were the 2:1 complexes (HPz3)2ZnBr2 (2) and (HPz6)2Zn(NO3)2 (3, HPzn = substituted pyrazole). Zinc perchlorate and tris(trimethylpy-razolyl)methane (L2) formed the octahedral binary complex [L22Zn](ClO4)2 (4) as evidenced by a structure determination. Zinc halides produced the 1:1 complexes L1 · ZnBr2 (5), L4 · ZnCl2 (6), and L4 · ZnBr2 (7), which according to the structure determinations of 6 and 7 contain tetrahedral ZnN2Hal2 units with only bidentate tris(pyrazolyl)methane ligands. In contrast, the zinc nitrate complex L4 · Zn(NO3)2 (8) was found to have an octahedral structure with mono- and bidentate nitrate and tridentate L4. The bromide complex 7 was converted by silver perchlorate hydrate into the labile compound [L4 · ZnBr]ClO4 (9) and then into the unstable product [L4 · Zn-OH2](ClO4)2 (10), both presumed to contain zinc in a tetrahedral ZnN3Br or ZnN3O environment, respectively. The ease of hydrolytic self-destruction prevented the exploitation of the reactivity of 9 and 10 in analogy to that of the corresponding tris(pyrazolyl)borate zinc complexes.
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    1,1-Hydroborierung von Alkinen mit 6-Aza-nido-decaboranen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 947-951 
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    ISSN: 0009-2940
    Keywords: 6-Aza-nido-decaborane ; 9-(1-Alkenyl)-6-phenyl-6-aza-nido-decaborane ; 1,1-Hydroboration of alkynes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,1-Hydroboration of Alkynes with 6-Aza-nido-decaboranes[1]Alkynes AC≡CR′ (R′ = Me, Bu, tBu, SiMe3), that contain a mobile group A, like H or SiMe3, undergo hydroboration by 6-aza-nido-decaboranes RNB9H11 (1a-c, R = H, Ph, PhCH2) and 1,2-migration of the group A, to give the corresponding 9-(1-alkenyl)-6-aza-nido-decaboranes RNB9H10(CH=CR′A) (2a-h). Ethenes AHC=CH2 (A = SiMe3, SnBu3) are hydroborated by 1a, b as well to form products of the type RNB9H10(CH2CH2A) (3a-c). The alkyne Me3SiC=CH undergoes a hydroboration with 1b twice; the formation of (PhNB9H10)2CHCH2SiMe3 (4) proceeds by a 1,1- and a 1,2-hydroboration step, apparently. The crystal structure analysis of (PhCH2)NB9H10[CH=CMe(SiMe3)] (2e; space group Pl) reveals a (Z configuration of the ethene moiety.
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    URL: http://dx.doi.org/10.1002/cber.19951280916
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    DBU - nicht einfach nur eine starke Base: Eine Eintopfreaktion für ein polycyclisches Ringgerüst mit Diphosphet - Grundstruktur unter Einbeziehung von doppelt deprotoniertem DBU (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 959-961 
    Details
    ISSN: 0009-2940
    Keywords: Nucleophilic behaviour of DBU ; Polyheterocycle ; Diphosphete ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: DBU - Not Simply a Strong Base: A One-Pot Synthesis of a Polycyclic Framework Consisting of a Diphosphete Central Unit and Two Units of Doubly Deprotonated DBUTwo condensed five-, six- and seven-membered rings are fused in a spirocyclic fashion with a central four-membered diphosphete ring in 4, which unexpectedly is formed in a simple two-component-one-pot reaction from Cl2P-CH(SiMe3)2 and DBU. The latter is doubly deprotonated and acts as a bridge via C-6 and N-8 to a P-P unit. The polyheterocycle 4 crystallizes in two modifications, whose molecular structures are almost identical.
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    URL: http://dx.doi.org/10.1002/cber.19951280919
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    The First Titanacyclic Five-Membered Cumulene. Synthesis, Structure, and Reactivity (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 967-971 
    Details
    ISSN: 0009-2940
    Keywords: Titanocene ; Diyne ; Cumulene ; Titanacyclopentadiene ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The first five-membered titanacyclic cumulene (5) was prepared by treatment of the titanocene generator Cp2Ti(Me3SiC2SiMe3) with the di-tert-butylbutadiyne in a molecular one-to-one ratio. The reaction of 5 with “Cp2Zr” or of the analogous complex with “Cp2Ti” leads to cleavage of the central C-C bond in the metallacyclocumulene complexes to afford the same product, the heterodimetallic ρ, π,-alkynyl-bridged titanocene-zirconocene complex Cp2Zr(μ-η1η2-C≡CtBu)Cp2Ti(μ-η1η2-C≡CtBu) (6), in which each alkynyl group is π-bonded to one and π-bonded to the other metal as shown by X-ray diffraction studies. In solution the two alkynyl groups become equivalent. The coupling reaction of “Cp2Ti” with bis(trimethylsilyl)butadiyne in a one-to-two molecular ratio leads to the unsymmetrically substituted titanacyclopentadiene (7).
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    Tri-tert-butylazadiboriridin: Ringerweiterung mit Isonitrilen, α-Bromlithioalkanen und Aziden (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1029-1035 
    Details
    ISSN: 0009-2940
    Keywords: Azadiboracyclobutanes ; Azadiboracyclopentanes ; Azadiboriridine, ring-opening of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tri-tert-butylazadiboriridine: Ring Prolongation by the Action of Isonitriles, α-Bromolithioalkanes, and AzidesIsonitriles ArNC are 1,1-boroborated by the B-B bond of the azadiboriridine (-BR-BR-NR-) (1; R = tBu) to form the four-membered ring [-BR-C(NAr)-BR-NR-] (2b; Ar = 2,6-C6H3Me2). Corresponding rings undergo [3 + 3] cyclodimerization of the B-C=N chain to give the tricyclic products 6a, b when isonitriles RNC with the small ligands R = Me, Et are boroborated by 1. Two molecules of tBuNC open the B-B bond of 1; the resulting five-membered ring 7a may add excess tBuNC to yield 7a · 2 CNtBu (8). The results strongly support a mechanistic hypothesis set up for the multistep reaction of 1 and CO. The carbene units, which are present in the α-bromolithioalkanes [-C(Br)Li-CMe2-CH2-], LiC(Br)H2, and LiC(Br)Me2, are also 1,1-boroborated by 1 to give the corresponding four-membered ring 2c, or by a 2:1 reaction to afford the five-membered ring 7b, or by a 1:1 reaction and subsequent rearrangement to yield the five-membered ring 7c. The nitrene units, which are present in the azides PhN3 and PhCH2N3, are also boroborated by 1; the diazadiboretidines 5b, c are formed with evolution of N2. The bis(diazadiboretidinyl)borane RB(N2B2R3)2 (5d) is the corresponding product from the reaction of RB(N3)2 with 1 in the ratio 1:2. The azide Me3SiN3 reacts differently yielding the N-boryl diazadiboretidine 5e and the iminoborane RB≡N̊. The B-B bond length of 187.6 pm in 5e indicates a transannular bonding interaction. The products 5d, 5e, and 6a were characterized by a crystal structure analysis.
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    Hypercoordinate Carbon in Trigoldbis(silyl)methanium Cations (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 137-142 
    Details
    ISSN: 0009-2940
    Keywords: Hypercoordinate carbon ; Gold(I) complexes ; Methanium cations ; Trigoldbis(silyl)methanium cations ; Gold clustering ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions of organolithium compounds of the type (R3Si)2CHLi (R3 = Me3 or Me2Ph) with the gold(I) complex Ph3PAuCl afford the monoaurated bis(silyl)methanes (R3Si)2- CHAuPPh3 (1a, b) in high yield. These compounds are converted into complex salts with hypercoordinate methanium cations {(R3Si)2C[Au(PPh3)]3}+BF-4 (3a, b) by treatment with {[(Ph3P)Au]3O}+ BF-4. In the reaction mixtures small amounts of the neutral dinuclear intermediates {(R3Si)2C[Au(PPh3)]2} (2a, b) have been detected and characterized by their spectroscopic data. Compounds 1a, b and 3a, b have been studied by single crystal X-ray diffraction analyses. While the mononuclear molecules 1a, b have conventional structures with parameters representing classical types of bonding, the novel trinuclear complexes 3a, b feature cations with a pentacoordinate carbon atom in a distorted trigonal-bipyramidal environment of two silicon atoms and one gold atom in equatorial positions and the remaining two gold atoms at the axial vertices of the polyhedra. The main axis of the bipyramid is strongly bent at the central carbon atoms. This distortion leads to short axial/equatorial Au…Au distances indicating peripheral metal-metal bonding.
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    Oxacycloalkenyliden-Komplexe von Chrom, Molybdän und Wolfram: Synthese, Anellierung mit Alkinen und Diels-Alder-Reaktionen mit Dienen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 157-161 
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    ISSN: 0009-2940
    Keywords: Carbene ligands ; Chromium complexes ; Molybdenum complexes ; Tungsten complexes ; Annulation reaction ; Diels-Alder reaction ; Oxacyclopentenylidene ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of Complex Ligands, LXI[1]. - Oxacycloalkenylidene Complexes of Chromium, Molybdenum, and Tungsten: Synthesis, Their Annulation with Alkynes and Diels-Alder Reaction with DienesLithiiated propargylic ether 1 reacts with M(CO)6 (M = Cr, Mo, W) to give the 2-oxacyclic carbene complexes 2-4 containing an α,β-double bond and a cyclic acetal structure which serves as a protected benzoyl group. Reaction of the chromium complex 2 with tolan leads to an acyl hydroquinone derivative 5. The tungsten complex 3 undergoes a [4 + 2] cycloaddition with cyclopentadiene to give two diastereomeric oxatricyclic carbene complexes 6 and 7 with an endo/exo selectivity of 3:1. The stereochemistry of the Diels-Alder reaction is controlled by the configuration of the acetal carbon center.
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    URL: http://dx.doi.org/10.1002/cber.19951280212
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    Stereospecific Ligand Substitutions in Manganese(I) Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 151-155 
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    ISSN: 0009-2940
    Keywords: Tripodal ligands ; Phosphane ligands ; Thioethers ; Manganese complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of fac-[(P2SPh-P,P')Mn(CO)3Br] and fac-[(PS2Ph-P,S)Mn(CO)3Br] [P2SPh: Z = PPh2; PS2Ph: Z = SPh in CH3C-(CH2PPh2)(CH2SPh)(CH2Z)] with silver hexafluorophosphate yields the η3-tripodal manganese complexes [(P2SPh-P,P',S)Mn(CO)3]PF6 (7) and [(PS2Ph-P,S,S')Mn(CO)3]PF6 (9), respectively, whereas the reaction of CH3C(CH2PPh2)2-(CH2SH) with Mn(CO)5Br gives directly [CH3C(Ph2-PCH2)2(CH2S)-P,P',S]Mn(CO)3 (11). Both ionic complexes 7 and 9 undergo stereospecifically ligand substitution upon treatment with Br-, I-, N-3, SCN- and CN- to give syn-fac-[(P2SPh-P,P')Mn(CO)3X] and syn-fac-[(PS2Ph-P,S)Mn(CO)3X] (X = Br, I, SCN, N3, CN) respectively, but the neutral complex 11 fails to undergo such a substitution reaction with these ions. However, reaction of I- with the complex [(PSMe)-P,P',S]Mn(CO)3]BF4 (20) [P2SMe = CH3C(CH2-PPh2)2(CH2SCH3)), which is obtained from the S-alkylation of 11 with (CH3)3OBF4, affords syn-fac-[(P2SMe)-P,P']Mn(CO)3I (22s) exclusively. The possible reaction mechanism of this ligand substitution is discussed.
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    Darstellung und Komplexierung von 1,4-Dimethyl-2,3-bis(isopropyliden)-1,4-diboratetralinHerrn Professor Nils Wiberg zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 183-185 
    Details
    ISSN: 0009-2940
    Keywords: 1,4-Diboranaphthalines ; 2,7-Diboradodeca-1,3,9,11-tetraenes ; Cobalt complexes ; Rhodium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Complexation of 1,4-Dimethyl-2,3-bis(isopropylidene)-1,4-diboratetraline1,4-Dimethyl-2,3-bis(isopropylidene)-1,4-diboratetraline (2) is obtained from o-dilithiumbenzene and 2,5-dimethyl-3,4-bis(chloromethylboryl)-2,4-hexadiene in 61% yield. Its complexation with cyclopentadienylbis(ethene)cobalt leads to the triple-decker bis(η5-cyclopentadienylcobalt)-μ-η6,η6-1,4-dimethyl-2-isopropenyl-3-isopropyl-1,4-dihydro-1,4-dibora-naphthaline (3) in low yield. However, the reaction of 2 with (C5H5)Rh(C2H4)2 and (C5Me5)Co(C2H4)2 originates complexes of a tricyclic ligand formed from 2 via conrotatoric [2 + 2] cycloaddition of the isopropylidene groups. (η5-Cyclo-pentadienylrhodium)-η6-tricyclo-[6.4.0.03,6]-2,4,4,5,5,7-hexamethyl-2,7-diboradodeca-1,3,9,11-tetraene (4), (η5-pentamethylcyclopentadienylcobalt)-η6-tricyclo-[6.4.0.03,6]-2,4,4,5,5,7-hexamethyl-2,7-diboradodeca-1,3,9,11-tetraene (5) and its related dinuclear complex 6 could be isolated in 29, 10, and 31%, respectively. Their constitutions are derived from spectroscopic data and proven by X-ray structure analysis of 4.
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    Pn-Liganden mit maximaler Elektronendonorfähigkeit, 7. Dreikomponentenreaktion von P4-Phosphor mit [CpxRh(CO)2] in Gegenwart von [Cr(CO)5THF] oder [CpMn(CO)2THF]. - Eine Methode zum Studium des Transformationsweges vom P4-Tetraeder zum planaren cyclo-P4-LigandenHerrn Professor Gerhard Fritz zum 75. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 251-257 
    Details
    ISSN: 0009-2940
    Keywords: Tetraphosphorus ligands ; Bond cleavage in P4, stepwise ; Rhodium P4 complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pn Ligands with Maximum Electron-Donor Capacity, 7. - Three-Component Reaction of P4-Phosphorus with [CpxRh(CO)2] in the Presence of [Cr(CO)5THF] or [CpMn(CO)2THF]. - A Method of Studying the Pathway from Tetrahedral P4 to the Planar cyclo-P4 LigandHerrn Professor Gerhard Fritz zum 75. Geburtstag gewidmet.The reaction of P4 with [CpxRh(CO)2] (Cpx = Cp′, Cp′′; Cp′ = η5-C5H4tBu, Cp′′ = η5-C5H3tBu2-1,3) in the presence of [Cr(CO)5THF] leads to [CpxRh(CO)(η1:1-P4){Cr(CO)5}4] (1a, b), [Cp′′Rh(η4-P4){Cr(CO)5}3] (2b), and [Cp′Rh(η4-P4){Cr-(CO)5}4] (3a). In the corresponding reaction with [CpMn-(CO)2THF] no P4 takes part, and [(Cp′′RhCO)(CpMnCO)(μ-CO)2] (4) is formed. An X-ray structure determination of [CpxRh(CO)(η1:1-P4){Cr(CO)5}4] (1) and [Cp′Rh(η4-P4)-{Cr(CO)5}4] (3a) indicates a stepwise (PP) bond cleavage as the transformation pathway from the P4 tetrahedron to the cyclo-P4 ligand by passing a bicyclotetraphosphane. In the cyclo-P4 ligand complex 3a all P atoms are able to coordinate to [Cr(CO)5] groups. However, in [Cp′′Rh(η4-P4){Cr(CO)5}3] (2b) the additional tBu group at the Cpx ligand sterically influences the coordination behavior of the P atoms, and only three of them are able to coordinate to [Cr(CO)5] units. In these syntheses the [Cr(CO)5] moieties promote the reaction and stabilise intermediates along the reaction pathway. Variable-temperature 31P{1H}-NMR measurements indicate for 2b the freezing of the Cp′′ rotation at low temperature and reveals a ΔG≠c (at the coalescence temperature) of 36 kJ mol-1. Surprisingly, in [(Cp′′RhCO)(CpMnCO)(μ-CO)2]-(Rh-Mn) (4) the Cpx ligands are cis-oriented whereas in [(Cp*RhCO)(CpMnCO)(μ-CO)2](Rh-Mn) a trans arrangement is observed. This indicates the unusual behavior of the Cp′′ ligand as a “rod” and not as an “enlarged disk” like Cp* in the crystal lattice of these compounds.
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    Darstellung von phosphor- und fluorhaltigen Calix[4]aren-Derivaten. Konformationsanalyse, Trennung der Konformere und Röntgenstrukturanalyse an einem KonuskonformerHerrn Professor Helmut Werner zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 267-273 
    Details
    ISSN: 0009-2940
    Keywords: Calix[4]arenes ; Supramolecular chemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Preparation of Phosphorus -  and Fluorine-Containing Calix[4]arene Derivatives. Conformational Analysis, Separation of the Conformers, and X-Ray Crystal Structure Analysis of a Cone ConformerHerrn Professor Helmut Werner zum 60. Geburtstag gewidmet.The Calix[4]arene 1 reacts with hexamethyldisilazane or (diethylamino)trimethylsilane to form the bis-trimethylsilyl-ated derivative 2. Treatment of 2 with PF2C1 gives the mono-and bis-difluorophosphites 3 and 4, which react with elimination of Me3SiF or PF3 to yield the monofluorophosphite derivative 5. All four OH hydrogen atoms in 1 are replaced by lithium on reaction with nBuLi with formation of the tetrali-thiated product 6. This has been allowed to react with the Pchlorophosphorinanones 7-9. From 7 the cone conformer 10a is formed, whereas in the case of 8 and 9 a mixture of all four possible conformars 11a-d and 12a-d is obtained. The pure conformers 12a-d are isolated. By refluxing the cone conformer 12a in tetrachloroethane a conformational conversion is effected. In order to evaluate its coordinating ability, 12a was allowed to react with dichloro(cycloocta-1, 5-diene)platinum(II) to form the trans-disubstituted complex 13. In the case of 12a (acetonitrile solvate) a single-crystal X-ray structure analysis has been conducted. The molecule displays a cone conformation, whereby two of the opposing phenyl rings are approximately parallel and the other two approximately perpendicular to each other.
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    Wasserlösliche Phosphane, IV. Tertiäre Alkylphosphane mit Ammoniumgruppen in den Seitenketten - Amphiphile mit basischen P-Atomen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 275-279 
    Details
    ISSN: 0009-2940
    Keywords: Aminoalkylphosphanes ; N-Quaternisation ; P-Alkylation ; Cationic tertiary phosphanes ; Amphiphiles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Water-Soluble Phosphanes, IV. - Tertiary Alkylphosphanes with Ammonium Groups in the Side Chains  -  Amphiphiles with Basic P-AtomsBy stepwise aminoalkylation of PH3 with Me2N—(CH2)2—Cl in the superbasic medium DMSO/KOH the secondary phosphane [Me2N—(CH2)2]2PH (2) is obtained in good yields. Metallation of 2 with n-BuLi and subsequent reaction with Me2N—(CH2)2]2Cl affords the basic tertiary phosphane [Me2N—(CH2)2]2]3P (3), which on protonation with Ph3P · HBr in CH2Cl2 gives {[HNMe2 - (CH2)2]3P}3+ 3 Br- (4a) with an extremely high solubility in water. By oxidation of 3 with H2O2 and N-quaternisation with Me3O+ BF-4 the cationic phosphane oxide {[Me3N—(CH2)2]3P=O}3+ 3 BF-4 (5a) is formed, which could, however, not be reduced with SiHCl3 or Si2Cl6/NEt3 to the corresponding tricationic phosphane. Tertiary cationic phosphanes of type [RMe2N—(CH2)2—P(Oct)2]+ X- (8a, 8b, R = Me, C8H17; X = Br, I) are accessible by free radical addition of 1-octene to 7b and 7d. Addition of formaldehyde to 7a gives the hydroxymethyl phosphane 10a. By methylation of [RMe2N—(CH2)2—PH2]+I- (7d and 7e, R = CnH2n+1, n = 8, 12) with Mel under controlled condition and subsequent deprotonation of the phosphonium salts 12b and 12c the cationic tertiary phosphanes 13a and 13b with long alkyl side chains may be obtained in good yields.
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    Charge-Transfer-Komplexe von Metalldithiolenen, XVIII. Ionenpaare von Dithiolencobaltaten mit Bipyridinium-Akzeptoren (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 303-307 
    Details
    ISSN: 0009-2940
    Keywords: Cobalt dithiolenes ; Charge-transfer complexes ; Electrical conductivity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Charge-Transfer Complexes of Metal Dithiolenes, XVIII. - Ion Pairs of Dithiolene Cobaltates with Bipyridinium AcceptorsIon pair charge-transfer (IPCT) complexes of the type {A2+[Co(mnt)2]2-}, mnt2- = cis-1,2-dicyano-1,2-ethenedithiolate, A2+ = a bipyridinium derivative, posses IPCT bands in the range from 590 to 950 nm. An X-ray structure analysis of {BQ2+[Co(mnt)2]2-}, BQ2+ = 6,7,8,9-tetrahydrodipyrido[1,2-a:2,1-c][1,4]diazocinium, reveals that the strongly twisted acceptor and planar donor do not form mixed stacks, as usually observed in less twisted systems. Electrical conductivities of pressed powder pellets are in the range of 10-15 to 10-7 Ω-1 cm-1 and do not exhibit a simple correlation with the driving force of electron transfer between the ion pair components. The cis-trans isomerization of an ethene-bridged methyl viologen acceptor leaves the conductivity almost unchanged.
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    Pentamethylcyclopentadienyl Iridium Complexes Containing Chalcogenido Ligands: Reactions of Cp*Ir(CO)2 with Elemental Sulfur and Selenium (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 557-560 
    Details
    ISSN: 0009-2940
    Keywords: Halfsandwich iridium complexes ; cyclo-Sulfido ligands ; Chalcogen-bridged iridium complexes ; Cubane clusters ; Iridium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Photolysis or thermolysis of Cp*Ir(CO)2 (1) in the presence of excess sulfur (S8) gives Cp*Ir(CO)(S4) (2a) which is further decarbonylated to [Cp*Ir(μ-S4)]2 (4a). The analogous reaction of 1 with excess selenium leads to Cp*2Ir2(μ-Se)(μ-Se4) (6b). In the case of limited chalcogen supply, the products are [Cp*Ir(CO)(μ-E)]2 [E = S (3a), Se 3b)] and [Cp*Ir(μ-E)]4 [E = S (5a), Se (5b)]. A stepwise formation of the pseudocubane clusters 5a,b from dinuclear precursors is assumed. The solid-state structure of 2a has been determined by X-ray crystallography.
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    URL: http://dx.doi.org/10.1002/cber.19951280605
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    Tin for Organic Synthesis, 12. Synthesis of Aromatic and Olefinic Sodium Sulfonates by Electrophilic Destannylation with Trimethylsilyl Chlorosulfonate (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 575-580 
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    ISSN: 0009-2940
    Keywords: Electrophilic aromatic substitution ; Electrophilic vinylic substitution ; Trialkylstannanes, application of ; Arylsulfonates, sodium salts of ; Vinylsulfonates, sodium salts of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A mild and effective method for the preparation of a variety of aromatic, olefinic, and acetylenic sodium sulfonates is described. The reaction of trialkylaryl- (2a-k) and -heteroarylstannanes (4a-d), bis-(1-alkenyl)dibutylstannanes (6a-f), or trialkylalkynylsta manes with trimethylsilyl chlorosulfonate (1) followed by hydrolysis with aqueous NaHCO3 provides the sodium sulfonates in an ipso-specific and in the case of vinylic stannanes stereospecific manner. A comparison of the reactivity of stannylated and silylated olefinic compounds 13 and 14 underlines the greater leaving ability of the stannyl moiety. The in situ preparation of the stannanes makes it possible to apply the synthetic method to natural products such as N-substituted apocodeine (17).
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    URL: http://dx.doi.org/10.1002/cber.19951280609
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    Soluble Substituted μ-Oxo(phthalocyaninato)iron(III) Dimers (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 589-598 
    Details
    ISSN: 0009-2940
    Keywords: μ-Oxobis(phthalocyaninato)iron ; μ-Oxo dimers ; Mössbauer spectroscopy ; Iron complexes ; Phthalocyanines ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Attempts to prepare various peripheral tetra- and octasubstituted (phthalocyaninato)iron derivatives RnPcFe [n = 4: R = CH2OEt (6e), CO2Et (6h), CO2-n-C6H13 (6l), O(2-Et-n-C6H13) (6j), OCH2C(CH3)3 (6k), OCH2C(CH3)2CH2Ph (6l); n = 8: R = CH2CH(CO2Me)CH(CO2Me)CH2 (6f), CH2CH(CO2Et)-CH(CO2Et)CH2 (6g), O-n-C8H17 (6m), O(2-Et-n-C6H13) (6n)] by starting from the corresponding substituted phthalonitriles led to substituted (μ-oxo)bis[(phthalocyaninato)iron(III)] compounds [RnPcFe]2O. The tert-butyl- and ethyl-substituted systems [tBu4PcFe]2O (6c) and [Et4PcFe]2O (6d) were reinve-stigated. UV/Vis, FD mass, Mössbauer, NMR as well as ESR spectroscopy was used to characterize the complexes [RnPcFe]2O to furnish evidence for the presence of Fe-O-Fe moieties in [RnPcFe]2O. The UV/Vis data reported for [RnPcFe]2O as well as their spectral behavior in pyridine correspond to unsubstituted [PcFe]2O. Mössbauer spectra of [RnPcFe]2O show that the complexes were obtained as a mixture of two isomeric μ-oxo compounds A (δFe = 0.22 mm s-1, ΔEQ = 1.33-1.39 mm s-1) and B (ΔFe = 0.33-0.36 mm s-1, ΔEQ = 0.39-0.53 mm s-1), whose Mössbauer parameters are comparable to [PcFe]2O μ-oxo(2) and μ-oxo(1), respectively. Mössbauer spectral data of [RnPcFe]2O indicate high-spin (S = 5/2) FeIII centers. NMR-spectra of [RnPcFe]2O (n = 4: R = tBu, Et, O(2-Et-n-C6H13), OCH2C(CH3)2CH2Ph; n = 8: R = O-n-C8H17, O(2-Et-n-C6H13) give further evidence for μ-oxo bridged structures.
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    Contributions to the Chemistry of Boron, 230Part 229: Ref.. Electrophilic Borylation of Metallocenes: Synthesis and Molecular Structures of 1,1′,3,3′-Tetrakis(dibromoboryl)metallocenes of the Iron TriadDedicated to Prof. Dr. Dr. h.c. Gerhard Fritz on the occasion of his 75th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 621-626 
    Details
    ISSN: 0009-2940
    Keywords: Ferrocene, tetrakis(dibromoboryl)- ; Ruthenocene, tetrakis(dibromoboryl)- ; Osmocene, tetrakis(dibromoboryl)- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of metallocenes MCp2 (M = Fe, Ru, Os) with an excess of BBr3 at reflux temperature lead specifically to 1,1′,3,3′-tetrakis(dibromoboryl)metallocenes 3, 7, and 8 in high yield. MeBBr2 and PhBBr2 are less effective borylating agents. X-ray structural analyses of 3, 7, and 8 reveal an increasing tilt of the Br2B groups towards the metal center while retaining the trigonal-planar environment at the boron atoms. This indicates a weak metal-boron interaction of the kind found for carbon-metal interactions in ferrocenyl carbocations.
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    Chirotopic and Stereogenic Metal Centers in [M(L)(L')(‘RS4’)] Complexes with Chiral Thioether-Thiolate Ligands ‘RS4’-H2 [‘MeS4’2- = 1,2-bis(2-mercaptophenylthio)propanato(2-), ‘CH3(CH2)2S4’2- = 1,2-bis(2-mercaptophenylthio)pentanato(2-), ‘HO(CH2)9S4’2-10 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 653-663 
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    ISSN: 0009-2940
    Keywords: Chirality ; Stereogenicity ; Diastereoselectivity ; Ligand stereospecificity ; Metal sulfur complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In order to investigate the stereochemistry of substitution reactions of chiral pseudo-octahedral complexes the chiral thioether-thiolate ligands ‘RS4’-H2 (= HSC6H4SCHRCH2-SC6H4SH) with R = CH3- (5), CH3(CH2)2- (6), HO(CH2)9- (7), and PhCH2- (8) were synthesized by template alkylation of Na2[Ni(‘S2’)2] [‘S2’2- = 1,2-benzenedithiolate(2-)] with 1,2-dibromoalkanes BrCHRCH2Br (R = CH3-, 1; R = CH3(CH2)2-, 2; R = HO(CH2)9-, 3; R = PhCH2-, 4) and isolated after hydrolyses. Reactions of ‘RS4’-H2 with [RuCl2(PPh3)3] or [Mo(O)2(acac)2] yielded [Ru(PPh3)2(‘RS4’)] (R = CH3-, 9; R = HO(CH2)9-, 10; R = PhCH2-, 11) and [Mo(O)2(‘MeS4’)] (12). [Ru(PPh3)2(‘MeS4’)] · 2 CH2Cl2 (9 · 2 CH2Cl2) and [Mo(O)2(‘MeS4’)] (12) were characterized by X-ray structure determination. In both complexes, the metal centers are surrounded pseudo-octahedrally by four sulfur donors of the ‘MeS4’ ligand and two cis coligands. The methyl substituent at the stereogenic C* atom of the C2 bridge of the ‘MeS4’ ligands assumes an equatorial position. In addition, the metal centers of these complexes are chirotopic and prostereogenic. Crystal data of 9 · 2 CH2Cl2 in comparison with [Ru(PBu3)2(‘S4’) 11-bis(2-mercaptophenylthio)-1-undecanolato(2-), ‘PhCH2S4’2-1,2-bis(2-mercaptophenylthio)-3-phenylpropanato(2-)] ] and those of 12 in comparison with [Mo(O)2(‘S4’)] show that distances and angles of the coordination cores are not influenced by the substituents on the C2 bridge. Reactions of the [Ru(PPh3)2(‘RS4’)] complexes (9-11) with the achiral substrates CO and PMe3, however, yielded diastereomers of [Ru(PPh3)(L)(‘RS4’)] (L = CO, R = CH3-, 13; L = CO, R = HO(CH2)9-, 14; L = CO, R = PhCH2-, 15; L = PMe3, R = CH3-, 16; L = PM R = HO(CH2)9-, 17; L = PMe3, R = PhCH2-, 18) in diastereomeric excesses between 60 and 82%. The diastereomer of [Ru(PPh3)CO)(‘MeS4’)] (13) which could be characterized by X-ray structure determination exhibits the CO ligand in trans position to the thioether donor which is bound to the stereogenic C* atom of the C2 bridge. Reaction of 9 · 2 CH2Cl2 with the optically pure bidentate diphosphine (+)-(S,S)-DIOP [= (+)-2,3-O-isopropylidene-2,3-dihydroxy-1,4-bis(diphenylphosphino)butane] yielded 1:1 mixtures of two diastereomers of [Ru(DIOP)(‘MeS4’)] (19) one of which was separated in pure form by HPLC.
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    A Deceiving X-ray Single-Crystal Structure Determination: Amino-Hydrogen Exchange in Amino-alkynylboranes and ab initio Investigations of Alkynylboranes, Borirenes, and Boraallenes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 711-717 
    Details
    ISSN: 0009-2940
    Keywords: Alkynylboranes ; Borirenes ; Boraallenes ; Calculations, ab initio ; Hydroboration ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Dimeric(dimethylamino)(phenylethynyl)borane (2)2 is formed by the reaction of bis(dimethylamino)(phenylethynyl)-borane (1) with 9-BBN-H. An X-ray single-crystal diffraction study revealed a central B2N2 four-membered ring for (2)2 with both alkynyl groups pointing to the same side in a cisoid arrangement. However, solution and solid-state NMR as well as ab initio calculations on model compounds show that the cis arrangement in the crystal chosen for X-ray diffraction is not representative of the bulk material, which consists of both cis and trans isomers. Further investigations of the competition between hydrogen-amino group exchange and hydroboration in the reaction of amino-alkynylboranes with hydroborating agents (9-BBN-H and catB-H) show the exchange to be much faster even in the presence of Wilkinson's catalyst and with cyclic amino-alkynylboranes such as 1,3-dimethyl-2-[(trimethylsily1)ethynyl]-1,3,2-diazaborolidine (3). Ab initio calculations on alkynylboranes I, borirenes II, and boraallenes III, which are all geometrical isomers, show alkynylboranes to be the most stable isomers only if strongly π-donating groups X (X = NH2, F) are attached to the boron atom. In any case, boraallenes are highest in energy.
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    URL: http://dx.doi.org/10.1002/cber.19951280709
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    Transition-Metal-Substituted Gallanes: Synthesis and Spectroscopic Studies of Highly Polar σ(M - Ga) Bonds, Structures of trans-(Ph3P)(CO)3Co - Ga[(CH2)3N(C 2H5)2]R (R = Cl, CH3) and (n5-C5H5)(CO)2Fe - GaCl2 [N(CH3)3]Dedicated to Prof. Hubert Schmidbaur on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 831-843 
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    ISSN: 0009-2940
    Keywords: Organogallium complexes ; Cobalt-gallium bonds ; Iron-gallium bonds ; MOCVD ; CoGa thin films ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The salt elimination reaction of the transition carbonyl metal-lates [L(CO)nM](Na/K) (M = Cr, Mo, W, Mn, Re, Fe, Co, Ni; L= CO, n5-C5R5, PR3; n= 1-4; R= alkyl, aryl) with the base-stabilized galliumhalides ClaGaR3 -a(Do) (R = H, alkyl, halide; Do = THF, N(CH3)3, NC7H13) or ClaGa[(CH2)3N-R2](R)2 - a yielded almost quantitatively the transition metal-substituted, gallanes [L(CO)nM]aGaR3 - a(Do) and [L(CO)n-M]aGa[(CH2)3NR2](R)2 - a, respectively. Residual halide functionalities in these complexes were selectively replaced by various other groups. The new compounds were characterized by means of elemental analysis, 1H-, 13C-, 31P-NMR, MS, and lR v(CO) data. The single-crystal X-ray structure analysis of trans-(Ph3P)(CO)3Co-Ga[(CH2) 3N(C2H5)2](R)( 6s: R = Cl, 6t: R= CH3) showed s̰(Co-Ga) lengths of 237.78(4) and 249.5(1) pm, respectively. A short s̰(Fe-Ga) contact of 236.18(3) pm was found for (n5-C5H5)(CO)2Fe-Ga-Cl2[N(CH 3)3] (5a). Low-pressure MOCVD experiments were performed to give thin films of analytically pure CoGa alloy.
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    URL: http://dx.doi.org/10.1002/cber.19951280815
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    Chiral Organometallic Reagents, XVI. Enantiomerization of α-Thio-, α-Seleno-, and α-Telluro-Substituted Alkyllithium Compounds; Kinetic and Mechanistic Studies (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 861-870 
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    ISSN: 0009-2940
    Keywords: Enantiomerization ; Organolithium compounds ; Dynamic NMR spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The rate of enantiomerization of the racemic α-phenylselenoalkyllithium compound 6 has been determined by dynamic NMR spectroscopy in [D8]THF. The enantiomerization rate was found to be first order with respect to monomeric 6 and to show no conspicuous solvent dependence (diethyl ether; toluene + 1 eq. of THF) or change upon addition of LiClO4. The marked steric effects on the enantiomerization rate found with the α-duryl- and α-mesityl-selenoalkyllithium compounds 7c and 7d suggest that rotation about the carbanion-selenium bond may be the rate-determining step in those sterically hindered systems. Similar steric effects were detected for the enantiomerization of the corresponding α-arylthio- and α-aryltelluroalkyllithium compounds 7j and 7f, but are absent with the α-arylsilyl-substituted alkyllithium compound 7o. This finding, along with the fact that the phenyltelluro- (7e), phenylseleno- (6), and phenylthio-alkyllithium compounds (7g) have essentially the same enantiomerization barrier, lead us to propose that in these cases a reorganization within the contact ion pair is the rate limiting step for the enantiomerization.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280903
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    Synthesis and Characterization of Copper(II) Complexes of a 14-Membered cis-N2S2 Dibenzo Macrocycle and of Its Bis-acetato and Bis(methylpyridyl) Derivatives (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1199-1205 
    Details
    ISSN: 0009-2940
    Keywords: Copper(I) complexes ; Copper(II) complexes ; N,S-Donor ligands ; Macrocyclic ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis and characterization of seven copper coordination compounds with the 14-membered macrocyclic cis-N2S2 dibenzo ligand 6,7,13,14,15,16,17,18-octahydrodibenzo[e,m]-[1,4,8,11]dithiadiazacyclotetradecine (L1) and its N,N'-bisacetato and -bis(methylpyridyl) functionalized derivatives H2L2 and L3 are described. The structures of five compounds were determined by single-crystal X-ray diffraction. The tetrahedrally distorted square-planar coordination geometry of [CuL1](ClO4)2 (1) changes upon reduction of copper to a severely distorted tetrahedral geometry in [CuL1]Br · MeCN (2). The Cu-N bond lengths increase from 1.988(3) to 2.029(5) Å; the Cu-S bond lengths decrease from 2.293(1) to 2.255(2) Å. Copper(II) is hexacoordinated in [CuHL2]HSO4 · 2.5 H2O (5) and [CuHL2]ClO4 · H2O (6). Both compounds exhibit very similar overall structures in the cationic part. The macrocyclic ring of the ligand is folded along an N⃜S axis, the octahedral geometry is strongly Jahn-Teller distorted, with O and S donor atoms in the apical positions. Compound 5 contains one very short [2.271(3) Å] and one long [2.701(3) Å] Cu-S (thioether) bond. In [CuL3](ClO4)2 · 2 H2O (7) one thioether group of the ligand L3 remains uncoordinated. The coordination polyhedron is rather irregular: Cu-S 2.506(3) and Cu-N 1.960(7)-2.107(8) Å. The compounds were further characterized by electronic and EPR spectroscopy and by cyclic voltammetry. Some relationships to the structural and spectroscopic properties of “blue” copper proteins were found.
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    URL: http://dx.doi.org/10.1002/cber.19951281211
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    New Pathways in Tellurium-Chalkogen-Nitrogen Chemistry: Preparations, Structures, and Properties of Telluraheterocycles (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 11-22 
    Details
    ISSN: 0009-2940
    Keywords: Thiaselenatelluradiazoles ; Thiaselenatelluratetrazocinium ; Tellurium(IV) compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of Se(NSO)2 with TeF4 in CH2Cl2 yields the compounds (4a) and (5b), while with TeBr4 after six months (2d) is formed. An almost quantitative yield of Cl4Te2N4S2 (6) is obtained from either Cl6Te2N2S (1a) and (CH3)3SiNSNSi(CH3)3 in CH2Cl2 at 20°C (2 d) or TeCl4 and (CH3)3SiNSO (molar ratio 1:2) in CH2Cl2 at 60°C (3 d). The use of (CH3)3SiOSi(CH3)3 as solvent in the last mentioned procedure gives 1a and small amounts of Cl2Te(NSO)2. Similarly, F2Te(NSO)2 is prepared from TeF4 and (CH3)3SiNSO in CH2Cl2. Dechlorination of 1a with (C6H5)3Sb leads to (2a), which is also produced from TeCl4 and [(CH3)3Si]2NSN[Si(CH3)3]2. When TeF4 is used instead of TeCl4 (molar ratio 3:1) the salt (7a) is formed. Similarly, (7b) is prepared from 2a and AsF5 or Ag+[AsF-6] in SO2. A new method for the preparation of bicyclic type 1 telluraheterocycles involves bromination of 2a yielding Cl2Br4Te2N2S (1b). Dehalogenation with (C6H5)3Sb converts 1b into (2b). When 2b is treated with Br2 in CH2Cl2 an oxidative halogenation takes place with formation of Br6Te2N2S (1c). Metathetical exchange between 2b and Ag+[AsF-6] gives (7c). Isostructural S(NSO)2 reacts with TeCl4 for several weeks at 60°C in CH2Cl2 to form S4N4. TeCl4 and [S5N+5][Te3Cl-3], in contrast to the corresponding reaction with Se(NSO)2. The molecular structures of 4a, 7b, 8, and [S5N+5][Te3Cl-13] have been determined by X-ray diffraction methods. Spectroscopic data for all new compounds are presented.
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    URL: http://dx.doi.org/10.1002/cber.19951280103
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