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  • Inorganic Chemistry  (83,665)
  • Computational Chemistry and Molecular Modeling  (8,042)
  • Wiley-Blackwell  (91,707)
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  • 101
    Electronic Resource
    Electronic Resource
    Darstellung und Kristallstruktur eines Kaliumnitridophosphats, K3P6N11 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 429-433 
    Details
    ISSN: 0044-2313
    Keywords: Potassium nitridophosphate ; synthesis ; 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 a Potassium Nitridophate, K3P6N11Single phase microcrystalline K3P6N11 was obtained by the reaction of P3N5 KNH2 in supercritical ammonia (6 kbr, 500°C) after 7 d reaction time in autoclaves. The structure was solved by X-ray powder diffraction methods. K3P6N11: P4132, a = 10.388(3) Å, Z = 4, RBragg (F02) = 0.087, 51 reflections K3P6N11 contains two- and three-fold corner-sharing tetrahedra PN4. These form a three-dimensional framework with potassium in voids coordinated by (2 + 6) N for K(1) and (3 + 3 + 3) N for K(2).
    Notes: Röntgenographisch phasenreines mikrokristallines K3P6N11 entsteht bei der Umsetzung von P3N5 mit KNH2 in Ammoniak unter ammonothermalen Bedingungen (6kbar, 500°C) nach 7d Reaktionszeit in Autoklaven. Die Struktur konnte über eine Röntgenstrukturanalyse am Pulver geklärt werden. K3P6N11: P4132, a = 10,388(3) Å, Z = 4, RBragg (F02) = 0,087, 51 Reflexe K3P6N11 ist aus zweifach- und dreifach eckenverknüpften Tetraedern PN4 aufgebaut, die ein dreidimensionales Gerüst bilden, in dessen Hohlräumen die Kaliumionen K(l) von (2 + 6) N von K(2) von (3 + 3 + 3) N umgeben sind.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230168
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  • 102
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstruktur von BaZn2(OH)6 · 5 H20 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 423-428 
    Details
    ISSN: 0044-2313
    Keywords: Barium hexahydroxodizincate pentahydrate ; synthesis ; crystal structure ; hydroxozincate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of BaZn2(OH)6 · 5 H2OThe electrochemical corrosion of zinc in a zinc/iron pair leads in an ammonia containing solution of barium hydroxide at room temperature to colourless platelets of crystals of BaZn2(OH)6 · 5H2O. The X-ray structure determination on these crystals was successful including all hydrogen positions: P21/c, Z = 4, a = 6.181(2) Å, b = 16.126(3) Å, c = 11.121(2) Å, β = 99.69(2)° Z(Fo2 ≥ 3 σ Fo2) = 3281, Z(Var.) = 178, R/Rw = 0.020/0.021 BaZn2(OH)6 · 5 H2O crystallizes in a layer structure. The layers contain Zn2+ in tetrahedral coordination by OH- and Ba2+ in an onefold capped tetragonal antiprism of 6 H2O and 3 OH-. Hydrogen bridge bonds of a further H2O molecule between the layers to OH- and H2O connect these three-dimensionally.
    Notes: Die elektrochemische Korrosion von Zink in einem Zink/Eisen-Paar führt in einer ammoniakalischen wäßrigen Lösung von Bariumhydroxid bei Raumtemperatur zu plättchenförmigen farblosen Kristallen von BaZn2(OH)6 · 5H2O. An ihnen wurde röntgenographisch die Struktur einschließlich aller H-Lagen bestimmt: P21/c, Z = 4, a = 6,181(2) Å, b = 16,126(3) Å, c = 11,121(2) Å, β = 99,69(2)° Z(Fo2 ≥ 3 σ Fo2) = 3281, Z(Var.) = 178, R/Rw = 0,020/0,021 BaZn2(OH)6 · 5H2O kristallisiert in einer Schichtstruktur. Innerhalb der Schichten ist Zn2+ tetraedrisch von OH- und Ba2+ einfach überkappt tetragonal antiprismatisch von 6H2O und 3OH- umgeben. Über Wasserstoffbrückenbindungen eines weiteren Moleküls H2Q zu OH- und H2O sind die Schichten dreidimensional verknüpft.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230167
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  • 103
    Electronic Resource
    Electronic Resource
    Kristallstruktur und Ramanspektrum von Nitroniumtrinitrosylpentanitratozirconat, NO2(NO)3[Zr(NO3)5]4Professor Roger Blachnik zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 449-455 
    Details
    ISSN: 0044-2313
    Keywords: Nitrosyl-Nitronium-Pentanitratozirconatenitrate ; Crystal Structure ; Raman Spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure and Raman Spectrum of Nitroniumtrinitrosylpentanitratozirconate, NO2(NO)3[Zr(NO3)5]4Single crystals of the triclinic compound NO2(NO)3[Zr(NO3)5]4 (a = 1376.3(6), b = 1376.9(11), c = 1632.0(7) pm, α = 114.63°(5), β = 114.90°(4), γ = 90.34°(5); P1, Z = 2) have been investigated by x-ray diffraction and Raman spectroscopy. The crystals were prepared by reaction of N2O5 with ZrCl4. The product was sublimed and crystallised in nitroethane.
    Notes: Einkristalle der triklinen Verbindung NO2(NO)3[Zr(NO3)5]4 (a = 1376,3(6), b = 1376,9(11), c = 1632,0(7) pm, α = 114,63°(5), β = 114,90°(4), γ = 90,34°(5); P1, Z = 2) wurden röntgenographisch und schwingungsspektroskopisch untersucht. Die Verbindung konnte durch Umsetzung von N2O5 mit ZrCl4, anschließender Sublimation und Umkristallisation in Nitroethan erhalten werden.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230172
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  • 104
    Electronic Resource
    Electronic Resource
    Darstellung und Kristallstruktur von LnCu4-xP2 (Ln: Y, La-Yb) sowie von LuCu3-xP2 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 608-612 
    Details
    ISSN: 0044-2313
    Keywords: Ternary copper phosphides ; yttrium ; rare earth ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of LnCu4-xP2 (Ln: Y, La-Yb) and LuCu3-xP2Several new ternary Cu phosphides were prepared by heating mixtures of the elements. The compounds LnCu4-xP2 (Ln: Y, La-Yb) crystallize in the rhombohedral CaCu4P2 type structure (R3m; Z = 3). Single crystal X-ray investigations of EuCu3.8P2, PrCu3.7P2 and GdCu3.7P2 (hexagonal axes see “Inhaltsübersicht”) confirmed this structure and revealed a deviation from full occupancy of one copper position. LuCu3-xP2 (R3m; Z = 6; a = 3.957(1), c = 40.109(3) Å; hex. axes) crystallizes in the YbCu3P2 type structure, which is derived from the CaAl2Si2 and Cu3P type structure.
    Notes: Durch Erhitzen entsprechender Elementgemenge konnte eine Reihe neuer ternärer Cu-Phosphide dargestellt werden. Die Verbindungen LnCu4-xP2 (Ln: Y, La-Yb) kristallisieren in der rhomboedrischen CaCu4P2-Struktur (R3m; Z = 3) mit einer geringfügig unterbesetzten Cu-Punktlage. Dies ergaben Strukturbestimmungen, die mit Einkristallmethoden an EuCu3,8P2 (a = 4,064(1), c = 22,762(2) Å), PrCu3,7P2 (a = 4,035(1), c = 22,318(4) Å) sowie GdCu3,7P2 (a = 3,994(1), c = 21,953(2) Å) (Gitterkonstanten jeweils in hexagonaler Aufstellung) durchgeführt wurden. LuCu3-xP2 (R3m; Z = 6; a = 3,957(1), c = 40,109(3) Å; hex. Aufstellung) kristallisiert im YbCu3P2-Typ, in dem sich längs [001] Baueinheiten abwechseln, die auf den CaAl2Si2- bzw. Cu3P-Strukturtyp zurückzuführen sind.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230195
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  • 105
    Electronic Resource
    Electronic Resource
    Darstellung und Strukturanalyse von Tetrakis-(N-Methylimidazolium)-silacyclopentandichlorid · 2 NMI (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 633-636 
    Details
    ISSN: 0044-2313
    Keywords: Tetrakis-(N-methylimidazolium)-silacyclopentane-dichloride · 2 NMI ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure Determination of Tetrakis-(N-Methylimidazolium)-silacyclopentanedichloride · 2 NMIThe reaction of 1,1-dichlorosilacyclopentane with N-methylimidazole in aprotic solvents leads to a 1 : 4 compound, stable at room temperature. The silicon-center of the resulting dication enlarges the coordination number from four to six. Therefore we find the chloride-ions removed from the first area of coordination. They have lost their bonding to the silicon atom. This species is the first Lewisacid/base compound consisting of a heterocyclic alkylsilicon-halide and a nitrogen-base. Two single NMI-molecules per dication are present in the unit cell with no coordination at all. That leads to an exact 1 : 6-ratio of silane to base.
    Notes: 1,1-Dichlorsilacyclopentan reagiert unter Anlagerung von vier N-Methylimidazol (NMI)-Molekülen in aprotischer Lösung zu einem sechsfach koordinierten Siliciumdikation, bie dem beiden Chloridionen aus der ersten Koordinationssphäre verdrängt werden. Hier liegt der erste Verbindungstyp eines Lewis-Säure/Lewis-Base-Adduktes bestehend aus einem heterocyclischen Alkylhalogensilan mit einer Stickstoffbase vor. Zwei weitere NMI-Moleküle befinden sich pro Dikation in der Elementarzelle, was einem exakten Verhältnis von Silan zu NMI von 1 : 6 entspricht.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301100
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  • 106
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    The Reaction of P3N3Cl4(NH2)2 with HCl; The Crystal Structure of P3N3Cl5(NH2) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 637-641 
    Details
    ISSN: 0044-2313
    Keywords: 2-amino-2,4,4,6,6-pentachloro-2λ5,4λ5,6λ5-cyclo-triphosphaza-l,3,5-trien ; 2,4-diamino-4,4,6,6-tetrachloro-2λ5,4λ5,6λ5-cyclotriphosphaza-l,3,5-trien ; 2,4-diamino-4,4,6,6-tetrachloro-2λ5,4λ5,6λ5-cyclotriphosphaza-l,3,5-trien-l-ium-chloride ; preparation ; crystal structure ; molecular structure ; vibrational spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die Reaktion von P3N3Cl4(NH2)2 mit HCl; Die Kristallstruktur von P3N3Cl5(NH2)P3N3Cl5(NH2) kann in hoher Reinheit und mit guten Ausbeuten durch Reaktion von P3N3Cl4(NH2)2 mit gasförmigem HCI in Acetonitril erhalten werden. Wird, Diethylether oder Dichlormethan als Lösungsmittel verwendet, scheidet sich die salzartige Verbindung [P3N3CI4H(NH2)2]+Cl als mikrokristallines Produkt aus. Die Kristallstruktur von P3N3Cl5(NH2) wurde durch Röntgen Kristallstrukturanalyse untersucht. Schwingungsspektren und thermisches Verhalten sowohl des P3N3Cl5 (NH2) als auch des [P3N3Cl4H(NH2)2]+Cl - werden kurz diskutiert.
    Notes: P3N3Cl5(NH2) in high purity and a good yield can be obtained by the reaction of P3N3Cl4(NH2)2 with gaseous HCl in acetonitrile. If diethylether or dichlormethane is used as a solvent, a salt-like compound [P3N3Cl4H(NH2)2]+Cl - is formed as a microcrystalline product instead of P3N3Cl5(NH2). The crystal structure of P3N3Cl5(NH2) was determined by X-ray structure analysis. Vibrational spectra and thermic behavior of both P3N3Cl5(NH2) and [P3N3Cl4H(NH2)2]+Cl - are also briefly discussed.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.199762301101
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  • 107
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    Metallkomplexe mit biologisch wichtigen Liganden. XCII. Hydridotrispyrazolylborato-Rhodium(III)-Komplexe mit α-Aminosäure-Anionen und PeptidenProfessor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 665-675 
    Details
    ISSN: 0044-2313
    Keywords: Hydridotrispyrazolylborate ; α-Aminocarboxylate ; Peptides ; Rhodium(III) Complexes ; X-ray diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal Complexes of Biologically Important Ligands. XCII, [1]. Hydridotrispyrazolylborato Rhodium(III) Complexes of α-Amino Carboxylates and PeptidesChiral chelate rhodium complexes Tp(Cl)RhNH2C(H)(R)CO2 and Tp*(Cl)RhNH2C(H)(R)CO2 (Tp = hydridotrispyrazolylborate, Tp* = hydridotris(3,5-dimethylpyrazolylborate)) were prepared and the ratio of diastereoisomers was determined. The diastereoisomers are remarkably stable towards eperimization. The reaction of [TpRhCl2]2 with glycineamide gives the ionic complex [Tp(Cl)Rh(NH2CH2CONH2)2]+ [TpRhCl3]- (15), whereas the reaction of Tp*Rh(Cl)2(HOMe) with glycine amide and di- and triglycine esters in the presence of NaOMe affords the neutral complexes 16-24, Tp*(Cl)2Rh(NH2CH2CONHR), Tp*(Cl)Rh(NH2CH2NR) and Tp*(Cl)Rh(NH2CH2CONCH2CONCH2CO2Me), respectively. Amidine complexes (25, 26) were obtained from TpRh(Cl)2(NCMe) and glycyl glycine esters by nucleophilic attack of the amino group to the carbon atom of coordinated acetonitrile. The structures of Tp*(Cl)Rh(L-alaO), Tp*(Cl)Rh(L-trpO), 15 and 25 were determined by X-ray diffraction.
    Notes: Die chiralen Rhodium-Komplexe Tp(Cl)RhNH2C(H)(R)CO2 und Tp*(Cl)RhNH2C(H)(R)CO2 (Tp = Hydridotrispyrazolylborat, Tp* = Hydridotris(3,5-dimethylpyrazolylborat)) wurden hergestellt und das Verhältnis der Diastereoisomeren wurde bestimmt. Die Diastereoisomeren sind bemerkenswert stabil gegenüber Epimerisierung. Die Reaktion von [TpRhCl2]2 mit Glycinamid liefert den ionischen Komplex [Tp(Cl)Rh(NH2CH2CONH2)2]+ [TpRhCl3] (15), während die Umsetzung von Tp*Rh(Cl) 2 (HOMe) mit Glycinamid und Di- und Triglycinestern die neutralen Verbindungen 16-24 ergibt. Amidin-Komplexe (25, 26) entstehen aus TpRh(Cl) 2 (NCMe) und Glycylglycinestern durch nucleophilen Angriff der Aminogruppe am Kohlenstoffatom des koordinierten Acetonitrils. Die Kristallstrukturen von Tp*(CI)Rh(L-alaO), Tp*(Cl)Rh(L-trpO) sowie von 15 und 25 wurden durch Röntgenbeugung bestimmt.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.199762301106
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  • 108
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    Synthese und Strukturuntersuchungen von Iodocupraten(I). XVII. Die Kristallstrukturen polymerer Iodo-thiocyanato-metallate(I) mit heterocubanartigen Baueinheiten: [(C2H5)4N+]2∞3[Cu4I4(SCN)4/22-] · 2(CH3)2CO und [(C2H5)4N+]2∞2[Ag 4I4(SCN)4/22-] · (CH3)2COProfessor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 687-694 
    Details
    ISSN: 0044-2313
    Keywords: Iodo-thiocyanato cuprate(I) ; Iodo-thiocyanato argentate(I) ; crystal structure ; heterocubane type anions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure Investigations on Iodocuprates(I). XVII. Crystal Structures of Polymeric Iodo-thiocyanato Metallates(I) with Heterocubane-like Structure Units: [(C2H5)4N+]2∞3[Cu4I4(SCN)4/22-] · 2(CH3)2CO and [(C2H5)4N+]2∞2[Ag 4I4(SCN)4/22-] · (CH3)2COThe reaction of CuSCN and AgSCN with (C2H5)4NI in acetone results in the formation of new Iodothiocyanato cuprates(I) or argentates(I) with polymeric anion lattices and areas of holes in which the cations and solvent molecules are inserted.[(C2H5)4N+]2∞3[Cu 4I4(SCN)4/22-] · 2(CH3)2CO 1 crystallizes in the monoclinic space group P21 with a = 1205.7(1), b = 2489.1(3), c = 1238.0(1) pm; β = 93.04(1)°; V = 3710.1(8) 106 pm3; Z = 2. Two different, negatively charged heterocubane units [Cu4I4(SCN)4/22-] are three-dimensionally connected by 1,3-μ-thiocyanato ligands forming a crystal structure with hose-shaped channels where cations and acetone molecules are placed.[(C2H5)4N+]2∞2[Ag 4I4(SCN)4/22-] · (CH3)2CO 2 crystallizes in the orthorhombic space group C2221 with a = 1206.7(1), b = 1398.2(1), c = 2318.8(2) pm; V = 3912.4(7) · 106 pm3; Z = 8. In this compound 1,3-μ-thiocyanato-bridged heterocubane units [Ag4I4(SCN)4/22-] form a layer structure with channel-shaped cavities vertical to them. Within these hollows there is again place for the cations and acetone molecules.
    Notes: Umsetzungen von CuSCN und AgSCN mit Tetraethylammoniumiodid in Aceton führen zu neuartigen, Iodo-thiocyanato-cupraten(I) bzw. -argentaten(I) mit polymeren Anionengittern, in deren Hohlräumen Kationen und Lösungsmittelmoleküle Platz finden.[(C2H5)4N+]2∞3[Cu 4I4(SCN)4/22-] · 2(CH3)2CO 1 kristallisiert in der monoklinen Raumgruppe P21; a = 1205,7(1), b = 2489,1(3), c = 1238,0(1) pm; β = 93,04(1)°; V = 3710,1(8) 106 pm3; Z = 2. Die Kristallstruktur ist aus zwei unterschiedlichen, zweifach negativ geladenen Heterocuban-Einheiten [Cu4I4(SCN)4/22-] aufgebaut. Diese sind über 1,3-μ-Thiocyanat-Liganden dreidimensional vernetzt. Zwischen den eckenverknüpften Heterocuban-Einheiten verlaufen schlauchförmige Kanäle, in denen sich die Kationen und Lösungsmittelmoleküle (Aceton) befinden.[(C2H5)4N+]2∞2[Ag 4I4(SCN)4/22-] · (CH3)2CO 2 kristallisiert in der orthorhombischen Raumgruppe C2221 mit den Zellparametern a = 1206,7(1), b = 1398,2(1), c = 2318,8(2) pm; V = 3912,4(7)· 106 pm3; Z = 8. In dieser Verbindung bilden 1,3-μ-SCN-verbrückte Heterocuban-Gruppen [Ag4I4(SCN)4/22-] polymere Schichten mit senkrecht dazu angeordneten, kanalförmigen Hohlräumen, in denen Kationen und Lösungsmittelmoleküle (Aceton) Platz finden.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301109
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  • 109
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    BaMgF4 and Ba2Mg3F10: New examples for structural relationships between hydrides and fluoridesDedicated to Professor Joachim Strähle on the Occasion of his 60th Birthday (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 705-709 
    Details
    ISSN: 0044-2313
    Keywords: Fluoride ; Synthesis ; Crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: BaMgF4 und Ba2Mg3F10: Neue Beispiele für Strukturverwandtschaften zwischen Hydriden und FluoridenBaMgF4 und Ba2Mg3F10 wurden durch Tempern stöchiometrischer Gemische der binären Fluoride synthetisiert und an Einkristalldaten verfeinert. BaMgF4 kristallisiert im orthorhombischen BaZnF4-Typ, Raumgruppe Cmc21 (Nr. 36), a = 4.126(1) Å, b = 14.518(4) Å, c = 5.821(2) Å, V = 348.7(2) Å3, Z = 4. Ba2Mg3F10 kristallisiert im monoklinen Ba2Ni3F10-Typ, Raumgruppe C2/m (Nr. 12), a = 18.495(2) Å, b = 5.9497(9) Å, c = 7.8187(9) Å, β = 112.04(1)°, V = 797.5(2) Å3, Z = 4. Die Strukturverwandtschaft zu den analogen Hydriden BaMgH4 und Ba2Mg3H10 wird diskutiert.
    Notes: BaMgF4 and Ba2Mg3F10 were synthesized by sintering stoichiometric mixtures of the binary fluorides and characterized by single-crystal X-ray diffraction. BaMgF4 crystallizes with the orthorhombic BaZnF4 structure type in space group Cmc21 (no. 36), a = 4.126(1) Å, b = 14.518(4) Å, c = 5.821(2) Å, V = 348.7(2) Å3, Z = 4. Ba2Mg3F10 crystallizes with the monoclinic Ba2Ni3F10 structure type in space group C2/m (no. 12), a = 18.495(2) Å, b = 5.9497(9) Å, c = 7.8187(9) Å, β = 112.04(1)°, V = 797.5(2) Å3, Z = 4. The structural relationships to their hydride analogues BaMgH4 and Ba2Mg3H10 are discussed.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301112
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  • 110
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    Koordinationsverhalten organometallischer Selenolato-Komplexe. Die Kristallstrukturen von [cp(CO)3W(μ-SeCH2Ph)W(CO)5], [cp(CO)3W(μ-SeCH2Ph)Cr(CO)5], [cp(CO)3W(μ-SeCH2Ph)Fe(CO)2cp]+ClO4- und [cp(CO)3W(μ-SeCH2SiMe3)AuPPh3]+SbF6-Professor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 735-741 
    Details
    ISSN: 0044-2313
    Keywords: Mononuclcar scfonolato tungsten complexes ; binuclear selenolato complexes ; 77Se-NMR ; x-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complexing Properties of Organometallic Selenolato Complexes. The Crystal Structures of [cp(CO)3W(μ-SeCH2Ph)W(CO)5], [cp(CO)3W(μ-SeCH2Ph)Cr(CO)5], [cp(CO)3W(μ-SeCH2Ph)Fe(CO)2cp]+ClO4-, and [cp(CO)3W(μ-SeCH2SiMe3)AuPPh3]+SbF6-The reaction of the selenolato tungsten complexes cp(CO)3WSeR; R = CH2Ph, CH2SeSiMe3, with the unsaturated complexes M(CO)5(THF); M = Cr, W or the complex cations Ph3PAu+ and cp′(CO)2Fe+; cp′ = C5H5, C5Me5, forms binuclear complexes, in which selenium possesses a formal positive charge. The crystal structures of the compounds 1, 2, 4 und 8 were determined by X-ray single crystal structure analysis (1: space group P212121 (Nr. 19), Z = 16, a = 1744.5(3) pm b = 2079.5(3) pm, c = 2435.7(5) pm; 2: space group P1 (Nr. 2), Z = 8, a = 1318.94(14) pm, b = 1732.5(2) pm, c = 2119.9(2) pm, = 89.805(10)°, β = 86.586(10)°, γ = 68.731(10)°; 4: space group P1 (Nr. 2), Z - 2, a = 828.0(5) pm, b = 1027.4(5) pm, c = 1510.8(9) pm, α = 109.84(3)°, β = 99.45(4)°, γ = 91,43(3)°; 8: space group P1 (Nr. 2), Z = 4, a = 1325.7(2)pm, b = 1663.1(3) pm, c = 1925.2(3)pm, α = 95.869(14)°, β = 103.091(12)°, γ = 112.871(10)°).
    Notes: Bei der Umsetzung der Selenolato-Wolfram-Komplexe cp(CO)3WSeR; R = CH2Ph, CH2SiMe3, mit den ungesättigten Komplexfragmenten M(CO)5(THF); M = Cr, W, bzw. den Komplexkationen Ph3PAu+ und cp′(CO)2Fe+; cp′ = C5H5, C5Me5, entstehen zweikernige Komplexe, in denen das Selenatom eine positive Ladung bzw. Partialladung trägt. Dabei konnten folgende Verbindungen charakterisiert werden: [cp(CO)3W(μ-SeCH2Ph)Cr(CO)5] (1), [cp(CO)3W(μ-SeCH2Ph)W(CO)5] (2), [cP(CO)3W(μ-p C6H4{CH2SeCr(CO)5}2)W(CO) 3cp] (3), [cp(CO)3W(μ-SeCH2Ph)Fe(CO)2cp]+ClO 4-, (4), [cp(CO)3W(μ-SeCH2Ph)Fe(CO)2cp*]+ClO4-, (5) [cp(CO)3W(μ-SeCH2Ph)AuPPh3]+SbF6- (6), [cp(CO)3W(μ-SeCH2Ph)AuPPh3]+ClO4- (7) und [cp(CO)3W(μ-SeCH2SiMe3)AuPPh3]+SbF6- (8). Die Strukturen der Verbindungen 1, 2, 4 und 8 konnten durch Einkristall-Röntgenstrukturanalyse aufgeklärt werden (1: Raumgruppe P212121 (Nr. 19), Z = 16, a = 1744,5(3) pm, b = 2079,5(3) pm, c = 2435.7(5) pm; 2: Raumgruppe P1 (Nr. 2), Z = 8, a = 1318,94(14) pm, b = 1732,5(2) pm, c = 2119,9(2) pm, α = 89,805(10)°, β = 86,586(10)°, γ = 68,731(10)°; 4: Raumgruppe P1 (Nr. 2), Z = 2, a = 828,0(5) pm, b = 1027,4(5) pm, c = 1510,8(9) pm, α = 109,84(3)°, β = 99,45(4)°, γ = 91,43(3)°; 8: Raumgruppe P1 (Nr. 2), Z = 4, a = 1325,7(2) pm, b = 1663,1(3) pm, c = 1925,2(3) pm, α = 95,869(14)°, β = 103,091(12)°, γ = 112,871(10)°).
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    Beiträge zur Kristallchemie der Urantelluride. IV [1, 2, 3]. Die Kristallstruktur von U0.9Te3Professor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 749-754 
    Details
    ISSN: 0044-2313
    Keywords: X-ray single crystal structure determination ; uranium telluride ; actinide chalcogenide ; nonstoichiometric compound ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Crystal Chemistry of Uranium Tellurides. IV. [1-3]. The Crystal Structure of U0.9Te3It is reported about the “β-modification” of the binary uranium polytelluride with the formula UTe3, which is thought to have a NdTe3-type structure, but which has been proved to be a nonstoichiometric compound with defects in the uranium partial structure and to be identical to a phase with the formula UTe3.38 already mentioned in the literature. As well the x-ray investigations of two single crystals as the analytical characterisation by EDX, ICP-OES and density measurements revealed an averaged composition of U0.9Te3 with a small phase width (0.87-0.93). As lattice parameters we found a = 435.37(3) pm, b = 2479.2(2) pm, c = 435.41(2) pm and a = 435.64(4) pm, b = 2481.8(2) pm, c = 435.96(4) pm, respectively, and as space group Cmcm (Z = 4). The cation positions of the NdTe3 structure type are depleted statistically in U0.9Te3. Super structure reflections as hints for an ordering of the defects were not observed. But the doubling and triplication of the unit cell dimensions in the direction of the layer sequence indicate the occurence of polytypic modifications.
    Notes: Berichtet wird über die „β-Modifikation“ des binären Uranpolytellurids der Formel UTe3, die im NdTe3-Typ kristallisieren soll, sich jedoch als nichtstöchiometrische Verbindung mit Defekten in der Uran-Partialstruktur und als identisch mit der in der Literatur erwähnten Phase der Formel UTe3.38 erwiesen hat. Sowohl die röntgenographischen Strukturanalysen an zwei Einkristallen sowie die analytische Charakterisierung mittels EDX, ICP-OES und Dichtemessungen ergaben eine mittlere Zusammensetzung von U0.9Te3 mit einer geringen Phasenbreite (0.87-0.93). Als Gitterparameter wurden a = 435.37(3) pm, b = 2479.2(2) pm und c = 435.41(2) pm bzw. a = 435.64(4) pm, b = 2481.8(2) pm und c = 435.96(4) pm gefunden, als Raumgruppe Cmcm (Z = 4). Die Kationenpositionen des NdTe3-Strukturtyps sind im U0.9Te3 statistisch unterbesetzt. Überstrukturreflexe als Hinweise auf eine Ausordnung der Defekte wurden nicht beobachtet. Jedoch zeigen Verdopplungen und Verdreifachungen der Elementarzelle in Richtung der Schichtabfolge das Auftreten von polytypen Modifikationen an.
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    Reaktionen von Zink- und Cadmiumhalogeniden mit Tris(trimethylsilyl)phosphan und Tris(trimethylsilyl)arsan Die Kristallstrukturen von [ZnI2{P(SiMe3)3}]2,[CdI2{P(SiMe3)3}]2,[NnBu4]2[Zn6I6(PSiMe3)4(C4H8O)2] · C6H6,[NnBu4]2[Cd4I8{P(SiMe3)2}2],[Zn4Cl4{P(SiMe3)2}4(MeCN)2],[Zn4Cl4{As(SiMe3)2}4(MeCN)2] und [Zn10Cl12(PSiMe3)4(PEt2Ph)4]Professor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 762-768 
    Details
    ISSN: 0044-2313
    Keywords: Zinc cluster ; Cadmium cluster ; crystal cluster ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Zinc and Cadmium Halides with Tris(trimethylsilyl)phosphane and Tris(trimethylsilyl)arsane The Crystal Structures of [ZnI2{P(SiMe3)3}]2,[CdI2{P(SiMe3)3}]2,[NnBu4]2[Zn6I6(PSiMe3)4(C4H8O)2] · C6H6,[NnBu4]2[Cd4I8{P(SiMe3)2}2],[Zn4Cl4{P(SiMe3)2}4(MeCN)2],[Zn4Cl4{As(SiMe3)2}4(MeCN)2] and [Zn10Cl12(PSiMe3)4(PEt2Ph)4]ZnI2 and CdI2 react with P(SiMe3)3 in diethylether resp. DME to the binuclear complexes [MI2{P(SiMe3)3}]2 (M = Zn 1, Cd 2). Further reaction of 1 with NnBu4I in THF leads to the formation of [NnBu4]2[Zn6I6(PSiMe3) 4(C4H8O)2]C6H6 3. 2 reacts with NnBu4I in THF to [NnBu4]2[Cd4I8{P(SiMe3) 2}2] 4.The reactions of ZnCl2 with P(SiMe3)3 resp. As(SiMe3)3 in MeCN at 0°C lead in a first step to the formation of the tetranuclear [Zn4Cl4{E(SiMe3)2}4(MeCN) 2] (E = P 5, As 6). The addition of the tertiary phosphine PEt2Ph to the reaction solution of ZnCl2 and P(SiMe3)3 in DME and subsequent layering with hexane results in the formation of [Zn10Cl12(PSiMe3)4(PEt2Ph) 4] 7.The structures of 1-7 were obtained by X-ray single crystal structure analysis (1: space group P212121 (Nr. 19), Z = 4, a = 1189.1 (2) pm, b = 1390.7(3) pm, c = 2550.7(5) pm; 2: space group P212121 (Nr. 19), Z = 4, a = 1499.5(3) pm, b = 1588.8(3) pm, c = 1813.5(4) pm; 3: space group Ibca (Nr. 73), Z = 8, a = 2365.5(5) pm, b = 2519.6(5) pm, c = 3118.7(6) pm; 4: space group Pna21 (Nr. 33), Z = 4, a = 1943.7(4) pm, b = 2032.9(4) pm, c = 2029.3(4) pm; 5: space group C2/c (Nr. 15), Z = 4, a = 2269.4(5) pm, b = 1471.5(3) pm, c = 1792.0(4) pm, β = 93.79(3)°; 6 space group C2/c (Nr. 15), Z = 4, a = 2262.4(5) pm, b = 1494.2(3) pm, c = 1801.1(4) pm, β = 90.30(3)°; 7: space group I41/a (Nr. 88), Z = 4, a = 2702.8(4) pm, b = 2702.8(4) pm, c = 1240.4(3) pm).
    Notes: ZnI2 und CdI2 reagieren mit P(SiMe3)3 in Diethylether bzw. DME zu den Zweikernkomplexen [MI2{P(SiMe3)3}]2 (M = Zn 1, Cd 2). 1 reagiert mit NnBu4I in THF unter Bildung von [NnBu4]2[Zn6I6(PSiMe3) 4(C4H8O)2]· C6H6 3. Dagegen erhält man aus 2 mit NnBu4I in THF den ionischen Cluster [NnBu4]2[Cd4I8{P(SiMe3) 2}2] 4.Die Reaktionen von ZnCl2 mit P(SiMe3)3 bzw. As(SiMe3)3 führen in MeCN bei 4°C in einer ersten Stufe zur Bildung der vierkernigen Zinkkomplexe [Zn4Cl4{E(SiMe3)2}4(MeCN) 2](E = P 5, As 6).Unter Verwendung eines tertiären Phosphans, PEt2Ph, lassen sich aus der Reaktionslösung von ZnCl2 mit P(SiMe3)3 in DME farblose kristalle des Mehrkernkomplexes [Zn10Cl12(PSiMe3)4(PEt2Ph) 4] 7 isolieren.Die Strukturen von 1-7 konnten durch Einkristall-Röntgenstrukturananlyse aufgeklärt werden. (1: Raumgruppe P212121 (Nr.19), Z = 4, a = 1189,1(2) pm, b = 1390,7(3) pm, c = 2550,7(5) pm; 2: Raumgruppe P212121 (Nr.19), Z = 4, a = 1499,5(3) pm, b = 1588,8(3) pm, c = 1813,5(4) pm; 3: Raumgruppe Ibca (Nr.73), Z = 8, a = 2365,5(5) pm, b = 2519,6(5) pm, c = 3118,7(6) pm; 4: Raumgruppe Pna21 (Nr.33), Z = 4, a = 1943,7(4) pm, b = 2032,9(4) pm, c = 2029,3(4) pm; 5: Raumgruppe C2/c (Nr.15), Z = 4, a = 2269,4(5) pm, b = 1471,5(3) pm, c = 1792,0(4) pm, β = 93,79(3)°; 6: Raumgruppe C2/c (Nr.15), Z = 4, a = 2262,4(5) pm, b = 1494,2(3) pm, c = 1801,1(4) pm, β = 90,30(3)°; 7: Raumgruppe I41/a (Nr.88), Z = 4, a = 2702,8(4) pm, b = 2702,8(4) pm, c = 1240,4(3) pm).
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    Se17[NbCl6]2 und Se17[TaBr6]2 - zwei neue Vertreter des Strukturtyps Se17[MX6]2Professor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 780-784 
    Details
    ISSN: 0044-2313
    Keywords: Heptadecaselenium(2+) ; Hexachloroniobate(-) ; Hexabromotantalate(-) ; solvothermal reactions ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Se17[NbCl6]2 and Se17[TaBr6]2 - Two New Compounds in the Structure Type Sel7[MX6]2The reaction of Se, SeCl4 and NbCl5 in SnCl4 in a sealed glass ampoule at 150°C yields Se17[NbCl6]2 and from Se, SeBr4 and TaBr5 in SiBr4 under the same conditions Se17[TaBr6]2 is formed. Both compounds crystallize triclinic in form of black moisture sensitive crystals, space group P1, Z = 2 (Se17[NbCl6]2: a = 1322.3(5) pm, b = 1309.0(6) pm, c = 1144.9(4) pm, α = 99.18(3)°, β = 99.55(3)°, γ = 112.17(3)°; Se17[TaBr6]2; 1354.5(7) pm, b = 1346.0(9) pm c = 1179.5(6) pm, α = 99.26(5)°, β = 97.81(4)°, γ = 112.52(5)°). Both are isotypic to the previously reported Se17[WCl6]2. The structures are built of octahedral [NbCl6] and [TaBr6] ions, respectively, and of (Se17)2+ ions The cations consist of two Se7 rings which are connected by a Se3 chain, and thus contain two three-coordinate Se atoms which carry formally the positive charge.
    Notes: Durch solvothermale Reaktion von Se, SeCl4 und NbCl5 in SnCl4 in einer geschlossenen Ampulle bei 150°C entsteht Se17[NbCl6]2 und aus Se, SeBr4 und TaBr5 in SiBr4 unter analogen Bedingungen Se17[TaBr6]2. Beide Verbindungen kristallisieren triklin in Form schwarzer, hydrolyseempfindlicher Kristalle, Raumgruppe P1, Z = 2 (Se17[NbCl6]2: a = 1322,3(5) pm, b = 1309,0(6) pm, c = 1144,9(4) pm, α = 99,18(3)°, β = 99,55(3)°, γ = 112,17(3)°; Se17[TaBr6]2: 1354,5(7) pm, b = 1346,0(9) pm, c = 1179,5(6) pm, α = 99,26(5)° β = 97,81(4)°, γ = 112,52(5)°) und sind isotyp zu Se17[WCl6]2 Die Strukturen sind aus oktaedrischen [NbCl6]- - bzw. [TaBr6]-- und aus (Se17)2+-Ionen aufgebaut, die aus jeweils zwei Se7-Ringen bestehen, die über eine Se3-Brücke verknüpft sind. Jedes Ion enthält zwei dreibindige Se-Atome, die formal die positive Ladung tragen.
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    Die Kristallstrukturen von CsBiO2 und Cs3BiO3Professor Joachim Strähle zum 60.Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 832-836 
    Details
    ISSN: 0044-2313
    Keywords: Cesiumbismuthate(III) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structures of CsBiO2 and Cs3BiO3CsBiO2 (pale yellow) and Cs3BiO3 (yellow) were obtained by solid state reactions of the binary components Cs2O und Bi2O3 at temperatures of 700°C and 550°C, respectively, The crystal structure of CsBiO2 (C2/c, a = 827.4(2), b = 920.4(2), c = 597.87(9) pm, β = 122.51(1)°, Z = 4, 975 diffractometer data, R1 = 0.058, wR2 = 0.077) contains infinite ∞1[BiO2/2O′2/2] chains. The structure determination of Cs3BiO3 (P213, a = 920,86(8), Z = 4, 289 diffractometer data, R1 = 0,048, wR2 = 0.081) reveals ‘isolated’ BiO33- groups. In this structure the cation arrangement is the same as that of the atoms in the intermetallic phase Cs3Bi.
    Notes: CsBiO2 (hellgelb) und Cs3BiO3 (gelb) wurden durch Festkörperreaktion aus den binären Komponenten Cs2O und Bi2O3 bei Temperaturen von 700°C bzw. 550°C dargestellt. In CsBiO2 liegen nach der Einkristallröntgenstrukturanalyse (C2/c; a = 827,4(2); b = 920,4(2); c = 597,87(9) pm; β = 122,51(1)°; Z = 4; 975 Diffraktometerdaten; R1 = 0,058; wR2 = 0,077) unendlich ausgedehnte ∞1[BiO2/2O′2/2]-Ketten vor. Die Kristallstruktur von Cs3BiO3 (P213; a = 920,86(8) pm; Z = 4; 289 Diffraktometerdaten; R1 = 0,048; wR2 = 0,081) enthält ‚isolierte‘ pyramidale BiO33--Anionen. Die Kationenanordnung in Cs3BiO3 entspricht der Atom-anordnung in der intermetallischen Phase Cs3Bi.
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    Novel dinuclear cyclometallated complexes of palladium(II) derived from N,N-(2,5-dichloro)terephthalylidenebis(cyclohexylamine) via oxidative additionDedicated to Professor Joachim Strähle on the Occasion of his 60th Birthday (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 844-848 
    Details
    ISSN: 0044-2313
    Keywords: Palladium ; Bidentate Schiff base ; Cyclometallation ; Oxidative Addition ; tertiary phosphine ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Neue Dinukleare Cyclometallierte Komplexe von Palladium(II) durch oxidative Addition mit N,N-(2,5-dichloro)terephthalylidenbis(cyclohexylamin)Die oxidative Addition der zweizähnigen Schiff-Base 1,4-(CyN=CH)2-2,5-CI2C6H2 an Tris(dibenzylidenaceton)dipalladium(0) ergab den dicyclopalladierten Komplex [(Cl)PdN(Cy)=C(H)C6H2C(H)=N(Cy)Pd(Cl)]n (1). Die Umsetzung von 1 mit LiBr ergab das analoge Bromoderivat [(Br)PdN(Cy)=C(H)C6H2C(H)=N(Cy)Pd(Br)]n (2). Reaktionen von 1 oder 2 mit tertiären Phosphinen in den Molverhältnissen 1:2 bzw. 1:4 führten zu den entsprechen den dinuklearen, cyclometallierten Komplexen [(L)(X)PdN(Cy)=C(H)C6H2C(H)=N(Cy)Pd(X)(L)] (3-9) und den nicht-cyclometallierten Komplexen [(L)2(X)PdN(Cy)=C(H)C6H2C(H)=N(Cy)Pd(X)(L)2] (10-14) (X = Cl, Br; L = PPh3, PEtPh2, PEt2Ph, PMePh2). Die Behandlung von 1 bzw. 2 mit Thalliumacetylacetonat führte zu dem dinuklearen, cyclometallierten Komplex [(MeCOCHCOMe)PdN(Cy)=C(H)C6H2C(H)=N(Cy)Pd(MeCOCHCOMe)] (15).
    Notes: The oxidative addition of the bidentate Schiff base 1,4-(CyN=CH)2-2,5-Cl2C6H2 to tris(dibenzylideneacetone) dipalladium(0) gave the dicyclopalladated complex [(Cl)PdN(Cy)=C(H)C6H2C(H)=N(Cy)Pd(Cl)]n (1). Treatment of 1 with LiBr gave the analogous bromo derivative [(Br)PdN(Cy)=C(H)C6H2C(H)=N(Cy)Pd(Br)]n (2). Reaction of 1 or of 2 with tertiary phosphines in 1:2 or 1:4 molar ratios gave the dinuclear cyclometallated [(L)(X)PdN(Cy)=C(H)C6H2C(H)=N(Cy)Pd(X)(L)] (3-9), and non-cyclometallated complexes [(L)2(X)PdN(Cy)=C(H)C6H2C(H)=N(Cy)Pd(X)(L)2] (10-14) (X = Cl, Br; L = PPh3, PEtPh2, PEt2Ph, PMePh2, as appropriate), respectively, Treatment of 1 or of 2 with thallium acetylacetonate gave the dinuclear cyclometallated complex [(MeCOCHCOMe)PdN(Cy)=C(H)C6H2C(H)=N(Cy)Pd(MeCOCHCOMe)] (15).
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    Synthese von cyclischen, chiralen Verbindungen mit Ge-El-Doppelbindungen (El = N, S, (O)) und deren dynamisches Verhalten in LösungProfessor Joachim Strähle zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 861-872 
    Details
    ISSN: 0044-2313
    Keywords: Germylene ; germaimine ; germathione ; oxydation of bis(amino)germylene by chalcogens ; reaction of a bis(amino)germylene with amine-N-oxide ; transient germanone ; X-ray structure analyses ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis of Cyclic, Chiral Compounds including Ge-El Double Bonds (El = N, S, (O)) and their Dynamic Behaviour in SolutionThe bis(amino)germylene 8, which can be synthesized by salt elimination reactions, reacts with trimethylsilylazid, elemental sulfur, and trimethylamine-N-oxide. The resulting chiral compounds 9 and 10 with Ge-N- and Ge-S-double bonds form in the solid state pairs of enantiomers, which can be proved by single crystal X-ray diffraction studies. Due to an intramolecular donor-acceptor bond between germanium and nitrogen atoms a bicyclus is formed, in which the germanium atom, a silicon atom and the donor nitrogen atom are chiral centers. In solution an equilibrium of diastereomers can be observed, resulting from an opening and closure of the donor-acceptor bondings of two concerning nitrogen atoms to the germanium atom. Depending upon the temperature the diastereomers show different dynamics in solution. A fluctioning germanium nitrogen double bond in 10 has been observed for the first time, which originates from a reversible silatrope migration of a trimethylsilyl group. By the reaction of the bis(amino)germylene 8 with trimethylamine-N-oxide first a transient germanone 11 a seems to form, which transforms to a germaimine 11 b by a migration of a trimethylsilyl group. This second intermediate is finally, adding a further molecule of trimethylamin-N-oxide to form 12.
    Notes: Über Salzeliminierungsreaktionen läßt sich das sterisch anspruchsvolle Bis(amino)germylen 8 darstellen, welches mit Trimethylsilylazid, elementarem Schwefel und Trimethylamin-N-Oxid umgesetzt wird. Die resultierenden chiralen Verbindungen 9 und 10 mit Ge-N- und Ge-S-Doppelbindungen liegen im Festkörper als Enantiomerenpaare vor, was durch Röntgenstrukturanalyse nachgewiesen werden konnte. Aufgrund einer intramolekularen Donor-Akzeptor-Bindung zwischen dem Germaniumatom und einem der Stickstoffatome kommt es zur Ausbildung eines Bicyclus, in dem das Germaniumatom. ein Siliziumatom und das Donor stickstoffatom asymmetrische Zentren darstellen. In Lösung entstehen durch Aufbrechen und Schließen der Donor-Akzeptor-Bindung in Konkurrenz mit dem zweiten Stickstoff-atom Diastereomere, die im Gleichgewicht miteinander stehen. Diese zeigen in Abhängigkeit von der Temperatur unterschiedliche dynamische Prozesse. Beim Germaimin 9 konnte hierbei zum ersten Mai eine „fluktuierende“ Ge-N-Doppelbindung beobachtet werden, was auf eine reversible silatrope Umlagerung einer Trimelhylsilylgruppe zurückzuführen ist. Das bei der Reaktion von 8 mit Trimethylamin-N-Oxid zuerst gebildete und als Intermediat zu formulierende Germanon 11 a, lagert sich durch Wanderung einer Trimethylsilylgruppe in ein Germaimin 11 b um, welches sofort ein weiteres Molekül Trimethylamin-N-Oxid unter gleichzeitiger Umlagerung addiert, was schließlich zu 12 führt.
    Additional Material: 12 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301136
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    Synthesis and crystal structure of M[Nb6Cl15] (M = In, Tl): New Ternary Niobium Halides with Bridged [Nb6Cl18]4- Clusters (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 908-912 
    Details
    ISSN: 0044-2313
    Keywords: In[Nb6Cl15] ; Tl[Nb6Cl15] ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Kristallstruktur von M[Nb6Cl15] (M = In, Tl): Neue ternäre Niobhalogenide mit verbrückten [Nb6Cl18]4- -ClusternDie neuen ternären Niobchloride M[Nb6Cl15] (M = In, Tl) wurden durch Festkörperreaktionen stöchiometrischer Gemische von NbCl5, Niobmetall und MCl3 bei 720°C dargestellt. Die Kristallstruktur von In[Nb6Cl15] wurde aus Einkristall-Röntgendaten bestimmt und in der orthorhombischen Symmetrie (Raumgruppe Pmma, Z = 4) mit a = 1786.6(1) pm, b = 1345,52(9) pm, c = 929,34(8) pm, R = 0,028, Rw = 0,037, GooF = 1,06 für alle symmetrieunabhängigen 1552 Reflexe verfeinert. Die Gitter-parameter der isotypen Verbindung Tl[Nb6Cl15] wurden aus Röntgen-Pulverdiffraktometerdaten verfeinert: a = 1785,9(2) pm, b = 1347,2(2) pm, c = 930,2(1) pm. Die Struktur besteht aus [Nb6Cl18]4--Clustern, die über terminale Chlorid-Liganden miteinander verbunden sind und zwei Sorten senkrecht zueinander stehender Ketten bilden, Diese Ketten sind über weitere terminale Liganden zu einem dreidimensionalen Netzwerk verbunden. Die In+- und Tl+-Ionen sind zehnfach koordiniert (in Form eines verzerrten zweifach bekappten Würfels), mit acht inneren und zwei äußeren Chlorid-Liganden.
    Notes: New ternary niobium chlorides corresponding to the formula M[Nb6Cl15] (M = In, T1) were synthesized from solid state reactions of NbCl5, niobium metal, and MCl3 at 720°C. The crystal structure of In[Nb6Cl15] was determined from single crystal X-ray diffraction studies. The structure was refined in the orthorhombic symmetry (space group Pmma, Z = 4) with a = 1786.6(1) pm, b = 1345.52(8) pm, c = 929.34(8) pm, RF = 0.028 and Rw = 0.037, GooF = 1.06 for all 1552 unique reflections. The lattice parameters of the isotypic Tl[Nb6Cl15] compound were refined from X-ray powder diffraction data: a = 1785.9(2) pm, b = 1347.2(2) pm, c = 930.2(1) pm. The structure of In[Nb6Cl15] is made up of [Nb6Cl18]4- clusters linked to each other through terminal chloride ligands to form two sets of chains perpendicular to each other. The chains are linked through other terminal ligands to yield a three-dimensional network. The In+ or Tl+ ions are located in a ten coordination site (distorted bicapped cubic geometry) made up of eight inner and two outer chloride ligands.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301143
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    [1,1,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5-diphosphet]trimethylaluminiuin und -indiumProfessor Walter Siebert zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 919-928 
    Details
    ISSN: 0044-2313
    Keywords: 1λ5, 3λ5-diphosphete ; aluminium ; indium complexes ; n.m.r ; mass ; ir spectra ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [1,l,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5-diphosphet]trimethylaluminiuin and -indium1,1,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5-diphosphet, 1, reacts with A1(CH3)3 and In(CH3)3 to give the complexes [l,l,3,3-tetrakis(dimethylamino)-1λ5, 3λ5-diphosphete]-trimethylaluminium, 2, and [1,1,3,3-Tetrakis(dimethylamino)-l,1λ5, 3λ55-diphosphete]-trimethylindium, 3, as crystalline products, respectively. Properties, n.m.r., mass and i.r. spectra are reported and interpreted. Compounds 2 and 3 are further characterized by X-ray structural analyses; the bonding situation in both complexes is discussed in detail
    Notes: 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet, 1, reagiert mit Al(CH3)3 bzw. In(CH3)3 zu den Komplexen [1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet]trimethylaluminium, 2, bzw. [1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet]trimethylindium, 3, die jeweils als kristalline Produkte erhalten werden. Die Eigenschaften, NMR-, Massen- und IR-Spektren werden mitgeteilt und interpretiert. 2 und 3 sind zusätzlich durch Kristallstrukturanalysen charakterisiert; die Bindungsverhältnisse in beiden Komplexen wurden eingehend diskutiert.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301145
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    Kristallstruktur, Schwingungsspektren und Normalkoordinatenanalyse von trans-(TEA)2[OsI4(CO)2] (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 937-940 
    Details
    ISSN: 0044-2313
    Keywords: Tetraiododicarbonylosmate(II) ; Crystal Structure ; Vibrational Spectra ; Normal Coordinate Analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis of trans-(TEA)2[OsI4(CO)2]The X-ray structure determination of trans-(TEA)2[Os(CO)2I4] (monoclinic, space group P21/n, a = 10.609(2), b = 10.659(3), c = 13.229(6) Å, β = 90.46(3)°, Z = 2) revealed the rough D4th point symmetry of the complex anion trans-[Os(CO)2I4]2- (Os—I = 2.726(1), 2.727(1); Os—C = 1.91(2); C—O = 1.14(2) Å). Using the molecular parameters the IR and Raman spectra are assigned by normal coordinate analysis. The valence force constants are fd(CO) = 15.86, fd(OsC) = 3.28, fd(OsI) = 1.13 mdyn/Å. The strengthening of the Os—C bond by stronger back donation of the OsII(d6) complex in comparison with the isostructural OsIII(d5) compound is discussed.
    Notes: Die Röntgenstrukturanalyse von trans-(TEA)2[Os(CO)2I4] (monoklin, Raumgruppe P21/n, a = 10,609(2), b = 10,659(3), c = 13,229(6) Å, β = 90,46(3)°, Z = 2) hat gezeigt, daß das centrosymmetrische Komplexanion trans-[Os(CO)2I4]2- (Os-I = 2,726(1), 2,727(1); Os-C = 1,91(2); C—O = 1,14(2) Å) annähernd D4th-Punktsymmetrie aufweist. Mit den röntgenographisch bestimmten Molekülparametern lassen sich die IR- und Raman-Spektren durch Normalkoordinatenanalyse zuordnen. Die Valenzkraftkonstanten betragen fd(CO) = 15,86, fd(OsC) = 3,28, fd(OsI) = 1,13 mdyn/Å. Die Festigung der Os—C-Bindung durch stärkere Rückbindung in dem OsII(d6)-Komplex im Vergleich zur isostrukturellen OsIII(d5)-Verbindung wird diskutiert.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301147
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    Phosphaniminato-Komplexe des Schwefels. Kristallstrukturen von [S(NPEt3)3]Cl, [S(NPEt3)2]Cl2 und [Me3SiOSO2NPPh3] (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 962-966 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes ; Sulfur Compounds ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorane Iminato Complexes of Sulfur. Crystal Structures of [S(NPEt3)3]Cl, [S(NPEt3)2]CI2 and [Me3SiOSO2NPPh3]The ionic phosphorane iminato complexes [S(NPEt3)3]Cl and [S(NPEt3)2]Cl2 are obtained as colourless, moisture sensitive crystals after reaction of Me3SiNPEt3 with disulfur dichloride from acetonitrile solutions. Both complexes, as well as the molecular complex [Me3SiOSO2NPPh3]. which is known from literature data, were characterized by crystal structure determinations.
    Notes: Die ionisch aufgebauten Phosphaniminato-Komplexe [S(NPEt3)3]Cl und [S(NPEt3)2]Cl2 entstehen als farblose, feuchtigkeitsempfindliche Kristalle nach Reaktion von Me3SiNPEt3 mit Dischwefeldichlorid in Acetonitrillösung. Beide Komplexe werden ebenso wie die literaturbekannte Molekülverbindung [Me3SiOSO2NPPh3] durch Kristallstrukturanalysen charakterisiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.199762301150
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    Photochemical reactions of transition metal organyl complexes with olefins, 17Part 16: Ref.. Light-Induced [6+2] Cycloadditions of Dienes to Tricarbonyl(η6-1,3,5,7-cyclooctatetraene)chromium(0) (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 9-12 
    Details
    ISSN: 0009-2940
    Keywords: Chromium ; Chromium(0) complexes ; Cyclooctatetraene complexes ; Photochemistry ; Cycloadditions ; Photochemical [6+2] cycloadditions ; Dienes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tricarbonyl(η6-1,3,5,7-cyclooctatetraene)chromium (1) yields upon UV irradiation in ether at 233 K with 2,3-dimethyl-1,3-butadiene (2) or 2-methyl-1,3-butadiene (3) by [6+2] cycloadditions the correspondingly substituted tricarbonyl(η6-bicyclo[4.2.2]deca-2,4,7-triene)chromium complexes 4, 5a and 5b. With ammonium cerium(IV) nitrate the organic ligand of complex 4, 9-isopropenyl-9-methyl-bicyclo[4.2.2]-deca-2,4,7-triene (6) is liberated. The complexes 4, 5a and 5b were characterised by IR and NMR spectroscopy, the ligand 6 by NMR spectroscopy.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300103
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    Characterization of a [4Fe-4S]-Ferredoxin Model Based on a Concave Tetradentate Thiol Ligand System (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 23-34 
    Details
    ISSN: 0009-2940
    Keywords: Cavitand ; Electrochemistry ; Iron sulfur cluster ; Metalloprotein model ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: NMR and Mössbauer spectroscopy show that a novel tetrathiol ligand, based on the cavitand diphenylglycoluril, encapsulates a 4Fe-4S cluster and induces asymmetry in it. The cluster gives a weak electrochemical current response in DMF, with a half-wave potential for the 2-/3- reduction vs. Fc+/Fc of -1.7 V. Ba2+ ions are adsorbed, according to X-ray analysis of the SEM image of the electrode, and act as modulator and promoter of the electrochemical response. On the basis of cyclic voltammograms it is proposed that this adsorption creates electroactive sites, changing the type of diffusion controlling the mass transport to the electrode from radial to linear, and that it helps the negatively charged complex, which contains a dipole, to approach the negative electrode in an orientation favourable for electron exchange. This feature makes the complex an important model for ferredoxins, in spite of a difference in redox potential.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300105
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    Generation and Synthetic Application of Metallated Methyl Isopropenyl Ether, A Substitute for Acetone Enolate (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 45-48 
    Details
    ISSN: 0009-2940
    Keywords: Metallated methyl isopropenyl ether ; Tetrahydrofurans ; 1-Oxabicyclo[4.3.0]heptanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Methyl isopropenyl ether (1) has been metallated at low temperature with a 1:1 molar mixture of n-BuLi/t-BuOK in THF-hexane, and subsequently functionalized with a variety of electrophilic reagents. At temperatures higher than - 30°C, the metallated methyl isopropenyl ether (2) decomposes with formation of allene. When the suspension of 2 is allowed to warm up to room temperature in the presence of an additional equivalent of n-BuLi, the intermediary allene is converted into 1-propynyllithium (2c), which reacts with propylthiocyanate to give 1-propylthio-1-propyne (4). Some of the functionalization products were subjected to acidic hydrolysis affording the expected methyl ketones.
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19971300107
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    Halogen/Metal vs. Hydrogen/Metal Exchange: General or Specific Site Selectivity as Exemplified in the Camphene Series (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 77-82 
    Details
    ISSN: 0009-2940
    Keywords: Monoterpenes ; Sesquiterpenes ; Stereoselectivity ; Alk-l-enyllithium(sodium) Metal exchange, halogen vs. hydrogen ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (Z)-(3,3-Dimethylbicyclo[2.2.1]hept-2-ylidene)methyllithium can be readily generated by treatment of (Z)-3-bromomethylene-2,2-dimethylbicyclo[2.2.1]heptane with tert-butyl-lithium. At -75°C, the organometallic intermediate is configurationally stable and reacts with a variety of electrophiles under stereochemical retention.
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    URL: http://dx.doi.org/10.1002/cber.19971300112
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    Conformational Mobility and Preferences of Allyl-Type Organometallic Intermediates: Dodec-2-enylpotassium (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 83-88 
    Details
    ISSN: 0009-2940
    Keywords: Torsional (Z/E) isomerization ; Selectivity, regio- and stereo- ; Allylsilanes ; Allylic oxidation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Alk-2-enylpotassium compounds having the endo conformation are synthetically very valuable precursors of (Z)-olefinic derivatives substituted at the outward allylic position. They may be generated by „stereoconservative‘ metalation of the readily available (Z)-alk-2-enes by using the superbasic mixture of butyllithium and potassium tert-butoxide or by metalation under similar conditions of stereorandom mixtures of alk-2-enes or alk-1-enes followed by torsional isomerization of the concomitantly formed exo conformers to the thermodynamically more stable endo species. The principal factors that dictate the rate and the extent of the endo/exo equilibration are the substrate geometry, the solvent, the temperature, the reagent stoichiometry, and catalysis.
    Additional Material: 5 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19971300113
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    Crown Thioether Chemistry: Novel Silver(I) Complexes of 1,3-Dithiole-Annelated 1,4,7-Trithiacyclononane (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 425-429 
    Details
    ISSN: 0009-2940
    Keywords: Silver complexes ; Crown compounds ; Thioethers ; 1,3-Dithioles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The coordination chemistry of two crown thioethers 2,5,8,10,12-pentathiabicyclo[7.3.0]dodeca-1)9)-ene-11-thione (L) and -11-one (L') with Ag1 has been investigated by structural methods. Both thioethers act as tridentate ligands coordinating the silver ion in a trigonal fashion. In the case L, the 11- thione sulfur is coordinated additionally by another silver ion, to yield a polymeric chain with a distorted-tetrahedral geometry about the metal ion. Despite differing only in its carbonyl chalcogen, L' forms six-coordinated, monomeric complexes.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300319
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    P/O Ligand Systems: Synthesis, Reactivity, and Structure of Tertiary o-Phosphanylphenol Derivatives (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 431-431 
    Details
    ISSN: 0009-2940
    Keywords: o-Phosphanylphenols ; P,O hybrid ligands ; P asymmetry ; C,O-dilithium reagents ; 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.19971300320
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    Molybdenum-Catalysed and -Mediated Cycloaddition Reactions: Efficient Synthesis of Complex Products from 1-Oxa-1,3-dienes and Cyclotrienes or -tetraenes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 453-462 
    Details
    ISSN: 0009-2940
    Keywords: Cycloadditions ; Catalysis ; 1-Oxa-1,3-dienes ; Molybdenum ; stereoselectivity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Molybdenum-mediated [6 + 2]-cycloaddition reactions of unsaturated ketones to cyclotri- or -tetraenes, e.g. cyclohepta-1,3,5-triene or cyclooctatetraene, proceed under very mild conditions, in high yields and with excellent stereoselectivity starting from the appropriate dicarbonylbis[π4-(1-oxa-1,3-diene)]molybdenum complexes. The stereochemistry of the product arising from the reaction of dicarbonylbis[π4-(5-methylhex-3-en-2-one)]molybdenum with cyclohepta-1,3,5-triene allows one to deduce a stepwise mechanism for this addition. The reactants are fused, as would be expected from an exo-type approach, thus indicating an intermolecular attack of the cycloheptatriene. Tungsten oxadiene complexes are effective in analogous reactions at somewhat reduced reaction rates. Catalytic cycloadditions are observed in several cases when 1-5 mol% of the highly reactive dicarbonylbis[π4-(R-(+)-pinocarvone)]molybdenum is employed as the catalyst. Cycloadducts are formed diastereospecifically in most cases. When cyclooctatrienes are employed as reactants, a sequence of electrocyclization of the triene and subsequent [4 + 2]-cycloadditon occurs with high selectivity and efficiency, leading to a pentacyclic ketone. The product structure reveals an endo-type approach of the polyene in this case.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300404
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    N2Hx Coordination at the Tripod-Cobalt Template CH3C(CH2PPh2)3Co: the Transformation of η2-HNNMe2 into η1-NNMe2Ligands (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 489-492 
    Details
    ISSN: 0009-2940
    Keywords: Nitrogenases ; Tripodal ligans ; Hydrazido ligands ; Side-on - end-on coordination ; Coordination modes ; Cobalt ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: While η2-coordination of N2H4 and N2H3- to tripod-cobalt entities has been reported, stabilization of N2H2 in this system has not yet been achieved. It is observed that [tripodCo(η2-HNNMe2)]+ (3) is transformed into [tripodCo(η1-NNMe2)]+ (4) by reaction with LiN(TMS)2 as a base. The deprotonation of 3 is accompanied by a redox reaction, and the overall reaction corresponds to the transformation of 3 to 4 with the loss of an electron and a proton. The observed coupling of deprotonation and oxidation is just the reverse of the processes assumed to occur during nitrogen fixation. The results are established by the usual analytical and spectroscopic techniques as well as by X-ray analyses.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300408
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    Highly Substituted Cyclams: Stereoselective Synthesis and Coordination Properties (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 521-528 
    Details
    ISSN: 0009-2940
    Keywords: Macrocycles ; Hydrogenation ; Cyclam, binding constant ; N ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: We report here a new synthetic route to highly-substituted tetraazamacrocycles. Raney nickel hydrogenation of macrocyclic phenylenediamine-acetylacetone condensation products gives cyclams in high yield with complexes all-cis stereoselectivity. The extensive C-substitution of the cyclam 2a changes its ligand properties markedly. The X-ray structure analyses of NiII, CuII, and ZnII complexes of 2a reveals a deviation of the metal ion coordination geometry from the usual square-planar arrangement. This may account for the differences in the redox properties of the NiII and CuII complexes of 2a leads to more positive oxidation and reduction potentials compared to the analogous unsubstituted cyclam complexes. While the binding constant between Zn(ClO4)2 and 2a is lower by a factor of 105 compared to cyclam, the subsequent binding of uridine to the zinc-cyclam complexes in methanol/water is slightly stronger in the case of 2a · Zn(ClO4)2].
    Additional Material: 6 Ill.
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    C-H Bond Activation of Simple Alkenes with (C5H5)CO Fragments: Preparation, Molecular Structure, and Dynamical Behaviour of Tri- and Tetranuclear Cyclopentadienylcobalt Cluster complexes with μ-Cycloalkyne Ligands (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 593-603 
    Details
    ISSN: 0009-2940
    Keywords: C-H activation ; Alkyne complexes ; Cyclopentadienyl cobalt ; Fluxionality ; Hydrido complexes ; Clusters ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Vicinal C-H bonds of the cycloalkenes CnH2n (n = 5-8) were activated upon treatment under mild conditions with reactive sources of the (C5H5)CO fragment. With [C5H5)CO(C2H4)2] (2a), the trinuclear cluster complexes [H2((C5H5)CO)3(μ3-C2(CH2)n-2)] (5a: n = 5; 5c: n = 5d: n = 8) were formed. Using the more reactive [(C5H5)2Co]/K, 5a-5dwere obtained, along with small amounts of the tetranuclear [{(C5H5)CO}4r{μ4-C2(CH2)n-2}] (8a-c: n = 5-7). X-ray structure analyses of 5c, d and 8b, c were performed. A μ-‖ (orμ3-η1:η2:η1) coordination of the cycloalkyne ligands was found in the trinuclear cluster complexes. The tetranuclear 8b, c had the cycloalkynes quadruply bridging (μ4-η1:η2:η2:η1_ a butterfly arrangement of the metal atoms. The acetylenic carbon-carbon bonds are considerably lengthened upon coordination [1.392(4), 1.398(3) å in 5c d; 1.464(8), 1.499(5) Å in 8b, c]. Three dynamic processes - alkyne “walk” on top of the CO3 triangle, μ2-hydride migration, and μ2/μ3-hydride exchange - are operational in the trinuclear 5a-d. Dynamic NMR data for 5a are consistent with a “windshield-wiper” mechanism for the alkyne migration. Hydride exchange is associated with a higher energy barrier, and is probably and independent dynamic process.
    Additional Material: 6 Ill.
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    Dynamic Behavior of Anionic Binuclear Helicate- and meso-Helicate-Type Coordination Compounds (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 615-619 
    Details
    ISSN: 0009-2940
    Keywords: Self-assembly ; NMR spectroscopy ; Titanium ; Catechol ligands ; Helical structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The racemization/symmetrization of helicate- or meso-helicate-type dinuclear titanium(IV) complexes Mn[(ligand)3Ti2] (n = 4: M = Li, Na, K, Cs; n = 2: M = Ca, Sr), which are formed by metal-directed self-assembly of alkyl-bridged bis(catecholate) ligands in the presence of basic alkali-metal or alkaline-earth metal salts, can be monitored by dynamic NMR spectroscopy. The free-energy barrier (ΔG
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    The Reactivity of Complexes of Nickel(0) and Platinum(0) Containing Benzyne and Related Small-Ring Alkynes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1029-1042 
    Details
    ISSN: 0009-2940
    Keywords: Nickel ; Platinum ; Aryne complexes ; Cyclohexyne complexes ; Insertions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation and reactivities of cyclohexyne and aryne complexes of platinum(0) and nickel(0) are reviewed. These complexes undergo insertions with unsaturated molecules such as alkenes, alkynes, isocyanides, CO and CO2. In the case of the nickel- benzyne complexes, consecutive insertions are observed with alkynes, leading to substituted naphthalenes with good regioselectivities. A possible mechanism for these double insertions, based on a combination of steric and electronic factors, is discussed in detail.
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    Synthesis and Structures of Sodium Phenylhydrazides (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1053-1062 
    Details
    ISSN: 0009-2940
    Keywords: Lithium ; Hydrazides ; Solvates ; Clusters ; Sodium ; Structure elucidation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Monomeric Li(Ph)N—N(Ph)SiMe3 · 2 OEt2 was obtained by deprotonating the respective hydrazine with nBuLi in the presence of diethyl ether. Reaction of NaN(SiMe3)2 with PhHN-N(SiMe3)2 in a benzene/tetrahydrofuran mixture provided monomeric Na(Ph)N—N(SiMe · 3 THF, or Nd(Ph)N—N(SiMe3)2 · THF using a small amount of THE Its TI IF ran be replaced by diethyl ether or tert-butyl methyl ether to give 1:l solvates. These associate, forming chains in the solid state via ηn coordination (n = 2, 3) of their phenyl groups to the sodium centers of adjacent molecules. In contrast, not only deprotonation but also desilylation occurs on reaction of NaN(SiMe3)2 with H(Ph)N—N(Ph)SiMe3 or of NaNH2 with (Me3Si)HN—NPh2) The latter reaction results in the formation ot hexameric (NaHN—NPh2)6 which adopts a face-sharing double-cubane structure.
    Additional Material: 10 Ill.
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    Characteristic Features of Neutral Cyclopropenylium-Like Compounds: Synthesis, Structure, and Chemical Behavior of a Cyclopropenylioborate Betaine (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1079-1084 
    Details
    ISSN: 0009-2940
    Keywords: Cyclopropenylium compounds ; Methylenecyclopropenes ; Isonitrile insertion ; Methylenecyclobutenone imine derivatives ; Cyclopropenylioborate betaines ; C-C coupling ; Zirconium ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bis(propynyl)zirconocene was treated with B(C6F.5)3 and then with two equivalents of tert-butyl isocyanide to yield the organometallic three-membered ring product 8. Subsequent hydrolysis gives the substituted (2-iminioethylidene)cyclopropeneborate betaine system 9 that exhibits a pronounced cyclopropenylioborate betaine character. This follows from its characteristic structural features (X-ray crystal-structure analysis of the isomer cis-9) and its chemical features. Complex 9 undergoes a very facile cis/trans isomerization by formal rotation around the exocyclic partial CC-double bond (ΔG+ ≈ 17 kcal mol-1). Compound 9 reacts cleanly in methanol solution with tert-butyl isocyanide by insertion and ring enlargement to form the four-membered ring system 12. Compound 12 was also characterized by X-ray diffraction.
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    Chiral Metal Carbene Modified [2.2]Metacyclophanes: Synthesis, Structure, and Chiroptic Properties (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1105-1111 
    Details
    ISSN: 0009-2940
    Keywords: Carbene complexes ; Chromium ; Cyclophanes ; Chirality ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pentacarbonyl(4-[2.2]metacyclophanyl(methoxy)carbene)-chromium(0) (6) was prepared according to the Fischer route from 4-bromo[2.2]metacyclophane. Aminolysis with non-chiral and chiral amines affords aminocarbene complexes 7-12. X-Ray structure analyses for 6 and its aminocarbene analogs 7 and 8 indicate that the incorporation of the chromium-carbene fragment has no significant influence on the deformation of the [2.2]metacyclophane skeleton.
    Additional Material: 5 Ill.
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    The Role of the 2,4,6-Tris(trifluoromethyl)phenylamino Group in Stabilizing New Phosphorus-, Arsenic-, and Germanium-Containing Main-Group Compounds and Transition-Metal Derivatives (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1113-1121 
    Details
    ISSN: 0009-2940
    Keywords: Phosphorus ; Arsenic ; Germanium ; Inorganic heterocycles ; Metal amides ; Fluorinated ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions of potassium Rf-amide [Rf = tris(trifluoromethyl)phenyl](2) with PCl3, AsC13, and GeC12 · dioxane yield new four-membered inorganic heterocycles [RfNPCl]2 (3), [RfNAsC1]2 (4), and [RfNGe]2 (5), respectively. On the other hand, the reaction of Rf-amide 2 with two equivalents of RfPCl2 leads to the formation of the imino-γ3-phosphane RfN=PRf (6) and the diamino-γ3-phosphane (RfNH)2PRf (7). The iminophosphane 6 reacts with Ni(CO)2(PPh3)2 and forms the complex [Ni(PPh3)2(RfN=PRf)] (9), in which the imino- phosphane coordinates to the metal through the phosphorus lone pair. Treatment of lithium amide 2 with transition metal chlorides ZnCl2 and FeCl2 yields the imido/amido spirocyclic metal derivatives 9 and 10, respectively. Compounds 3-10 have been extensively characterized by their analytical and mass, IR, and NMR (1H, 19F, and 31P) spectroscopy. Further, the molecular structures of all the compounds have been unambiguously determined by single-crystal X-ray diffraction studies. The diazadigermetidine 5 crystallizes in a fluorescent-yellow orthorhombic and a yellow monoclinic crystal modification. The results obtained reveal the role of Rf, group in stabilizing new multiple bonded systems and inorganic heterocycles. A skeletal rearrangment of the Rf ligand is observed in the reactions leading to compounds 9 and 10. Moreover, the preparation of compounds 9 and 10 indicates the limitation of the use of this ligand in the preparation of new metal-amide systems, especially where the metal atoms have a strong tendency for the formation of strong M—F bonds.
    Additional Material: 8 Ill.
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    Organophosphorus Compounds, 114. Tetracyclic Phosphorus-Aluminium-Carbon Compounds - Synthesis by Cooligomerization of Kinetically Stabilized Phosphaalkynes with Trialkylaluminium CompoundsDedicated to Professor Michael Hanack on the occasion of his 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 255-259 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkynes ; Triorganoaluminium compounds ; Cooligomerization ; Cage compounds ; Aluminium compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: When the trialkylaluminium reagents 5 are allowed to react with phosphaalkynes 4 in n-pentane, a highly selective phosphaalkyne cyclotrimerization with incorporation of two organometallic units occurs (→ 6). The tetracyclooctane derivatives 6a-e represent the first examples of phosphorus-aluminium-carbon cage compounds. The polycyclic products 6 are able to function as ligands in transition-metal complexes (→ 7), which is illustrated by the reactions of 6b, c with nonacarbonyldiiron and pentacarbonyl(tetrahydrofuran)tungsten, respectively.
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    URL: http://dx.doi.org/10.1002/cber.19971300219
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    On the Ligating Properties of Sulfonate and Perchlorate Anions Towards Zinc (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 283-289 
    Details
    ISSN: 0009-2940
    Keywords: Zinc ; Sulfonate ligands ; Perchlorates ; Coordination modes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Attempts are reported to incorporate sulfonate and perchlorate anions as ligands in zinc complexes of tripodal ligands. Using tris(benzimidazolylmethyl)amine (BIMA) only the aqua complexes [ (BIMA)Zn-OH2](RSO3)(ClO4) and [(BIMA)Zn-OH2](RSO3)2(R=CH3, CF3, p-tolyl) were accessible. Using substituted pyrazolylborates (Tp*), the same three sulfonate anions were found to be ligands in the complexes Tp*Zn-OSO2R. Spectroscopic evidence for perchlorate coordination in Tp*ZnClO4 · 2 DMSO conflicts with crystallograpic evidence against it in Tp*ZnClO4 · pyridine. The crystal structures of [(BIMA)Zn-OH2](CH3SO3)2, TpCum,MeZn-OS02CH3, TPtBu,MeZn-OSO2C6H4-p-CH3, and [TpCum,MeZn · NC5H5]ClO4 were determined.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300223
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    Preparation of Methyl 2-[Bis(trimethylsiloxy)phosphoryl]-3,3,3-trifluoro-2- (trimethylsiloxy)propionate and Some Derivatives-Molecular Structure of Methyl 2-[Bis(trimethylsiloxy)phosphoryl]-3,3,3-trifluoro-2-hydroxypropionate (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 279-281 
    Details
    ISSN: 0009-2940
    Keywords: Methyl trifluoropyruvate ; Tris(trimethylsilyl) phosphite ; Methyl 2-[bis(trimethylsiloxy)phosphoryl]-3,3,3- trifluoro-2-(trimethylsiloxy)propionate ; Bis(trimethylsilyl) [(2,2-difluoro-l-trimethylsiloxy)ethenyl]- phosphonate ; Solid-state structures ; Fluorine ; Phosphorus ; Silicon ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Methyl trifluoropyruvate (1) and tris(trimethylsilyl) phosphite (3) reacted to give methyl 2-[bis(trimethylsiloxy)phosphoryl]- 3,3,3-trifluoro-2-(trimethylsiloxy) propionate (4). Partial hydrolysis furnished propionate 6, the molecular structure of which was obtained in the solid state. Attempted trimethylsilylation of the methylcarboxylato group in 4 using iodotrimethylsilane caused the formation of bis(trimethylsily1) [(2,2- difluoro- 1 -trimethylsiloxy)ethenyl]phosphonate (8). For comparison, methyl pyruvate (2) and 3 gave methyl 2-[bis(trimethylsiloxy)phosphoryl]-2-(trimethylsiloxy)propionate (5).
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300222
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    1,4,7,10,13,16,19,22-Octaazacyclotetracosane-1,4,7,10,13,16,19,22-octaacetic Acid (H8OTEC) and 1,4,7,10,14,17,20,23-Octaazacyclohexacosane- 1,4,7,10,14,17,20,23-octaacetic Acid (H8OHEC): Synthesis and Characterization of Two Large Macrocyclic Polyamine Polycarboxylic Ligands and Some of Their Copper(II) and Lanthanide(III) Complexes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 267-277 
    Details
    ISSN: 0009-2940
    Keywords: Macrocyclic ligands ; Lanthanides ; Copper ; Polyamines ; Polycarboxylic acids ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The optimized synthesis of two new macrocyclic polyamine polycarboxylic ligands, 1,4,7,10,14,17,20,23-octaazacyclohexacosane-1,4,7,10,14,17,20,23-octaacetic acid (H8OHEC) (10) and 1,4,7, 10,13,16,19,22-octaazacyclotetracosane-1,4,7,10, 13,16,19,22-octaacetic acid (H8OTEC) (12), is presented. The key step in the synthesis of both is the high yield carboxymethylation of the corresponding macrocyclic amines using tert-butyl bromoacetate followed by acidic hydrolysis of the acetate protecting groups. The molecular structures of the intermediates 1,4,7,10,14,17,20,23-octaazacyclohexacosane (OHEC-amine) (8), and octa-tert-butyl 1,4,7,10,13,16,19,22- octaazacyclotetracosane-1,4,7,10,13,16,19,22-octaacetate (OTEC-ester) (11) are determined by X-ray crystal structure analysis. OHEC-amine 8 reacts with 2 equiv. of CuSO4 yielding the dinuclear complex [Cu2(OHEC-amine)](SO4)2 (13). Complex 13 crystallizes with 16 molecules of water. 13 · 16 H2O contains two copper atoms, which are coordinated in a strongly distorted octahedral fashion by four nitrogen atoms, one oxygen atom from the sulfate dianion and one oxygen atom from a water molecule. The new ligands 10 and 12 are fully characterized by 1D- and 2D-NMR spectroscopy. Both ligands form dinuclear lanthanide(III) chelates (Ln=Y, Sm, Eu, Gd, Yb, Lu), which are stable and highly water soluble. With lanthanum(III) only mononuclear complexes are formed.
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    Multiple Bonds Between Main-Group Elements and Transition Metals, CLXIV. Alkylrhenium(VI) Oxides-Synthesis and Characterization (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 295-298 
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    ISSN: 0009-2940
    Keywords: Rhenium ; Oxides ; Alkyl ligands ; Dirhenium compounds ; Metal-metal interactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Most alkylrhenium(VII) oxides, e.g. ((cyclo)-C3H5)Re03 (2) are rather sensitive to temperature and moisture with the prominent exception of methyltrioxorhenium (1). The corresponding alkylrhenium(VI) oxides of formula [RR′(O)- Re(μ-O)]2 [R=R′=(cyclo)-C3H5 (3), iPr (4); R=CH3, R′=C2H5 (5), R=CH3, R′=iPr (6)] are much more stable in this regard. They can be handled in air at room temperature. They were synthesized from Re207 and dialkylzinc precursors, fully characterized and are available in much higher yields than their ReVII congeners. Mixed tetraalkyltetraoxodirhenium(VI) complexes (R # R′) synthesized from 1 and dialkylzinc compounds form as a mixture of cis/trans isomers. They are oily liquids at room temperature. The Re=O and Re-Re stretching force constants as a measure of the bond strengths, were determined from IR and Raman data.
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    URL: http://dx.doi.org/10.1002/cber.19971300225
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    Reactions of Complex Ligands, LXXIIPart LXXI: Ref. [1].Intermolecular Pauson-Khand Reactions of Ethyl 2-Phenylethynylcyclopropanecarboxylates and [Amino(trans-2-phenylethynylcyclopropyl)methylidene]pentacarbonylchromium(0)Dedicated to Professor Dr. G. E. Herberich on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 507-514 
    Details
    ISSN: 0009-2940
    Keywords: Carbene complexes ; Chromium ; Cycloadditions ; Cyclopropanecarboxylic and derivatives ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The intermolecular Pauson-Khand reactions of ethyl trans-2-phenylethynylcyclopropanecarboxylate (1t) and [amino-(trans-2-phenylethynylcyclopropyt)methylidene]pentacarbonylchromium (9) with norbornane lead to ester and metal carbene functionalized exo-tricyclodecenones 3b-6 and 13-16, respectively, in moderate to high yields. The incorporation of the alkyne is moderately regioselective but less diastereoselective. Pairs of diastereomers are isolated after column chromatography, which can subsequently be separated by recrystallization. The minor diastereomer 3 and the major diastereomer 15 are characterized by X-ray structure analysis.
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    Masthead (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997) 
    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.19971300501
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    Inter- and Intramolecular Thermal Activation of Aliphatic C-H Bonds Mediated by Complexes Containing the Fragments [{Cy2P(CH2)nPCy2}M] (n=1-4, M = Rh, Ru) (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 555-558 
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    ISSN: 0009-2940
    Keywords: C-H activation ; Homogeneous catalysis ; Dehydrogenation ; Phosphane complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A well defined geometrical structure and a well established catalytic potential for a plethora of processes puts the chelate rings [{R2P〈(CH2)nPR2}M] (M = Rh, Ru) among the most interesting candidates for catalytic alkane functionalization in homogeneous solution. It is demonstrated that intermolecular thermal C-H activation (3→4) is possible with readily accessible complexes [{Cy2P(CH2)nPCy2}Rh(hfacac)] (n = 1-4, 1a-c and [Cy2P(CH2)nPCy2}Ru(η3-C4H7)2] (n = 1-3, 2a-c) containing such fragments. A maximum of 5 catalytic cycles was achieved with complex 2a. In case of Ru complexes containing the same ligands with n =3 and 4, intramolecular cleavage of three adjacent C-H bonds in one of the cyclohexyl substituents at phosphorus also occurs readily leading to formation of a new polydentate k2P,P', η3-allyl ligand.
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    URL: http://dx.doi.org/10.1002/cber.19971300504
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    Layered Ternary and Quaternary Metal ChalcogenidesDedicated to Prof. Dr. Hans Georg von Schnering on the occasion of his 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1-8 
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    ISSN: 0009-2940
    Keywords: Chalcogenides ; Reactive flux ; Layered compounds ; Structures ; Physical properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The syntheses, crystal structures, and physical properties of some recently discovered layered ternary and quaternary chalcogenides are reviewed. One component of these systems is an alkali metal or thallium; another is a d-, f-, or p- block metal.
    Additional Material: 12 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300102
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    Synthesis of Functionalized Carbamates through a Palladium-Catalyzed Reductive Carbonylation of Substituted Nitrobenzenes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 13-22 
    Details
    ISSN: 0009-2940
    Keywords: Carbamates ; Catalysis ; Substituted nitrobenzenes ; Palladium ; Reductive carbonylation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The palladium-catalyzed reductive carbonylation of ortho and para-substituted nitrobenzenes has proven to be an attractive route for the synthesis of functionalized carbamates. For the Pd(1, 10-phenanthroline)2(triflate)2 catalyst system, the scope of the reaction has been studied. Substrates with electron-donating substituents at the para position were found to decrease the catalytic activity, most probably as a result of their relatively low oxidizing capacity. the selectivity towards the desired carbamate, however, was increased for these substrates. Under the influence of electron-withdrawing substituents the azoxybenzene and azobenzene derivatives became important side products. Introduction of large steric hindrance at the ortho position of the nitro substrates gave rise to an interesting side reaction, viz. methoxylation of the aromatic ring. The methoxylation reaction appeared to occur on an intermediate species in the catalytic cycle. Several functionalities have shown to be resistant to the reaction conditions required for the conversion ot the nitro group. Especially with 4-nitrobenzoic acid, an extremely high activity and selectivity was found, thus yielding a very convenient synthesis for N-protected amines containing carboxylic acid function.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300104
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    Atropisomeric Binaphthalene-Core Phosphacyclic Derivatives in Coordination Chemistry and Homogeneous Catalysis (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 543-554 
    Details
    ISSN: 0009-2940
    Keywords: Phosphorus heterocycles ; Binaphthophosphole ; Atropisomerism ; Binaphthophosphepine ; Hydroformylations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Binaphthophospholes and binaphthophosphepines have recently been synthesized. These are the first representatives of a new class of chiral ligands that include within the same structure an endocyclic phosphorus donor, a local C2 symmetry and an axially chiral core. In this review we discuss the synthesis, chemical behaviour and first applications in asymmetric catalysis of these novel derivatives.
    Additional Material: 4 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19971300503
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    Iminoacylcobalt Compounds as Starting Materials for the Synthesis of Alkynylcobalt Halfsandwiches and CobaltaheterocyclesDedicated to Professor Günter Schmid on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 565-570 
    Details
    ISSN: 0009-2940
    Keywords: Cobalt ; Cycloadditions ; Heterocycles ; Alkynyl complexes ; Cyclopentadienyl complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The iminoacylcobalt compound [C5H5Co(C(CH3)=NCH3)(PMe2Ph)] (3) reacts with propargylic acid ester HC=CCO2R (R = Me, Et) to give the alkynylcobalt halfsandwich-type complexes [C5H5Co(C(CH3)=NHCH3)(C=CCO2R)-(PMe2Ph)]I (5, 6). With HC=CCO2Me as the substrate, besides 6 (R = Me) the five-membered cobaltaheterocycle [C5H5Co{K2(N, C)-N(CH3)C(CH3)CHC(CO2Me)}(PMe2Ph)]I (7) is also obtained. The reactions of 3 and the analogous benzyl derivative 4 with terminal alkynes HC=CR' (R' = CH2OH, CMe2OH, [CH2]2OH, CH2OMe, H, Me, nBu, Ph) afford exclusively the heterocyclic complexes [C5H5Co(K2(N,C)-N(R)C(CH3CHCR')(PMe2Ph)]I (R = CH3, CH2Ph) (8-18) in 60-70% yield. The molecular structures of 5 (R = Et) and 16 (R = Me, R' = Ph) have been determined by X-ray crystallography.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300506
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    The First Electron-Donor-Acceptor Paracyclophanes with Ferrocene NLO-Phores: Synthesis, Absorption and Electrochemical Properties (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 581-584 
    Details
    ISSN: 0009-2940
    Keywords: Vinylferrocene ; Pd-catalyzed twofold and fourfold couplings ; Electron-donor-acceptor[2.2]paracyclophanes ; Charge transfer ; Cyclic voltammetry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: As potential nonlinear optical material. 12-nitro-4,7-bis(2-ferrocenylvinyl)[2.2]paracyclophane (1) and 12-nitro-4,5,7,8-tetrakis(2-ferrocenylvinyl)[2.2]paracyclophane(2) have been synthesized by pd-catalyzed coupling reactions of vinylferrocene with the precursor cyclophanes 9 and 13, respectively. The absorption and electrochemical properties of 1 and 2 are also described.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19971300508
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    Gold Coordination by 2-(Diphenylphosphanyl)aniline (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 647-650 
    Details
    ISSN: 0009-2940
    Keywords: Gold(I) coordination ; 2-(Diphenylphosphanyl)aniline ; Ambidentate P ; N ligands ; P Ligands ; Ligand effects ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of 2-(diphenylphosphanyl)aniline (1) with (tetrahydrothiophene)gold(I) chloride in the molar ratio 1:1 gives a stable molecular complex 2, in which the gold atom is bonded to the phosphorus atom. Reaction of two equivalents of ligand 1 with one equivalent of the salt [(tht)2Au]ClO4 results in the displacement of both thioether ligands, affording the ionic complex {[(2-NH2C6H4)PPh2]2Au}+ ClO-4 (3a), in which the metal center is exclusively P-coordinated. Treatment of [(tht)2Au]ClO4 with ligand 1 (1:1) affords the mixed P/S-coordinated complex 4, the structure of which has been confirmed by single-crystal X-ray diffraction. The reaction of ligand 1 with [(Ph3P)Au]+ BF-4 leads to a mixture of products which are components of an equilibrium between the unsymmetrical salt {[(2-NH2C6H4)PPh2]Au(PPh3)} BF-4 with the two symmetrical species 3b (the BF-4 analogue of 3a) and [(Ph3P)2Au]+ BF-4, With {[(Ph3P)Au]3O}+ BF-4 as the aurating agent, the ligand 1 (molar ratio 1:1) is converted into a polynuclear complex 7, which is tentatively assigned a structure with intimate aggregation of six gold atoms.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300516
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    On the Protonation of Fluoro Cryptands and the Possibility of CF…HN+ Hydrogen Bonds (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 633-640 
    Details
    ISSN: 0009-2940
    Keywords: Fluorine ; Macrocycles ; Cryptands ; Protonations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The protonation of several fluoro cryptands synthesized from 1,3-bis(bromomethyl)-2-fluorobenzene and diaza-macrocycles (diaza-12-crown-4, diaza-15-crown-5, diaza-18-crown-6 and 2,3-benzodiaza-15-crown-5) has been investigated by 1H-, 13C- and 19F-NMR spectroscopy, X-ray crystal structure analysis and IR spectroscopy, with a view to detecting possible CF…HN hydrogen bonding. From the crystal structures of mono- and diprotonated 23-fluoro-4,7,20-trioxa-1,10-diazatricyclo[8,7,5,112,16]tricosa-12,14,16(23)-triene (FN2O3·H+ and FN2O3·2H+) it is apparent that protonation leads to a shortening of the non-bonded nitrogen-fluorine and nitrogen-oxygen distances and consequently to O·HN hydrogen bonds. A related type of interaction involving fluorine appears possible since short N(H)…F distances (281.2-286.6 pm) with NHF angles between 130-140° are observed. A Cambridge Structural Database search was performed and 27 structures with short CF…HN contacts were found. On the other hand, IR spectra do not give any clear evidence in favor of CF…HN hydrogen bonding since the N-H vibrations in FN2O3…H+ and FN2O3…2H+ as well as in FN2O4…2H+ do not experience longwave shifts relative to the N-H vibrations of the reference systems HN2O3·H+, HN2O3…2H+ and HN2O4…2H+.HN2O3 and HN2O4 are almost identical to FN2O3 and HN2O4, respectively, the only difference being that the single fluorine atom of the fluoro cryptands is replaced by hydrogen. NMR spectroscopic evidence concerning CF…HN interactions is ambiguous: (i) A spin-coupling between 1H and 19F (NH…F) is observed. (ii) The 1JCF value is reduced by up to 15 Hz upon protonation of the fluoro cryptand. (iii) An NMR competition experiment between FN2O3 and HN2O3 yields no evidence for an increased basicity of the fluoro cryptand. Finally, it can be stated that evidence in favor of CF…HN hydrogen bonds is inconclusive; should such an interaction exist it will certainly be very weak.
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    URL: http://dx.doi.org/10.1002/cber.19971300514
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    Monomeric Phosphanylgalanes  -  Synthesis and Structural Characterization (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 663-668 
    Details
    ISSN: 0009-2940
    Keywords: Phosphanylgallanes ; Gallium amino compounds ; P Ligands ; Gallium ; Ab initio calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The monomeric phosphanylgallanes R2GaPR'R (R = tmp, Mes; R' = H, tBu; R' Mes, tBu), the diphosphanylgallane mesGa(PtBu2)2, and diphosphandiylbisgallane [tmp2GaP-(tBu)]2, have been synthesized from alkali metal phosphides and substituted gallium chlorides. Low-temperature NMR studies of the phosphanylgallanes reveal no barrier to rotation about the gallium-phosphorus bond. Analysis of the crystal structures of tmp2GaPtBu2 confirms the monomeric nature of these molecules. The gallium-phosphorus bond lengths are found to be 237.5, 233.5, 235.4 pm (averaged), and 242.3 pm, respectively, with all phosphorus atoms being pyramidally coordinated.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300519
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    Fully Chlorinated N-Silyl Amides of Titanium and Tungsten  -  Crystal Structure of Cl3SiNW(Cl3)N(SiCl3)2 (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 701-704 
    Details
    ISSN: 0009-2940
    Keywords: N-Silyl amides ; Precursor ; 14N-NMR ; Titanium ; Tungsten ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of hexachlorodisilazanyllithium (Cl3Si)2NLi (1), with TiCl4 leads selectively to the novel fully chlorinated amides (Cl3Si)2NTiCl3 (2) or [(Cl3Si)2N]2 TiCl2 (3), respectively, depending on the molar ratio of the starting materials. The analogous reaction of 1 with WCl6 yielded the amide imide Cl3SiN=W(Cl3)N(SiCl3)2 (5) by elimination of SiCl4. The relative amounts of the starting materials had no effect on the formation of 5. 14/15N- and 29Si-NMR data on the starting materials and products show significantly different effects, when compared with those of analogous N-trimethylsilyl derivatives, due to the lower energy of the electrons in the N—Si and N—M ß bonds. The crystal structure of 5 (triclinic, space group P1) was determined by X-ray structure analysis.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300605
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    Well-Defined Metallodendrimers by Site-Specific Complexation (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 725-728 
    Details
    ISSN: 0009-2940
    Keywords: Dendrimers ; Metal complexes ; Nanostructures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Strong multiple complexation of transition metal ions, Cu(II), Zn(II) and Ni(II) with different generations of well-defined poly(propylene imine) dendrimers as multi(tridentate) ligands has been used to construct nanoscopic assemblies of defined structure and size incorporating a distinct number of metal ions from 2 up to 32.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300608
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    Synthesis of Germatranyl Derivatives of Esters of Carboxylic Acids via Organometallic (Si, Ge, Sn) Reagents (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 739-746 
    Details
    ISSN: 0009-2940
    Keywords: Germatranes ; Organotrihalogenogermanes ; Organometallic (Si, Ge, Sn) reagents ; Transmetallation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trialkylstannyl esters of tris(2-hydroxyalkyl)amines, N(CH2CHROSnAlk3)3 (9-11 (R = H, Me; Alk = Et, Bu), react with X3GeC(R1)(R2)COOR3 (12-17) (X = Cl or Br; R1, R2=H, Me, Ph, SiMe3, COOEt; R3=Me, Et) to give esters of α-germatranylcarboxylic acids, N(CH2CHRO)3GeC(R1)(R2)-COOR3 (1-8), in high yields. The synthesis of esters 12-17 is reported. Esters of α-germatranyldiphenylacetic acid 24 and 25 can be obtained by treatment of diphenylketene with Et3SnOMe to give in situ Et3SnC(Ph2)COOMe (23), followed by reaction with GeCl4 to give in situ Cl3GeC(Ph2)COOMe (22 and further reactions with 9 or 11, respectively. Reduction of germatrane 6 with LiAlH4 in diethyl ether leads to cleavage of the germanium-carbon bond with subsequent formation of (2-hydroxyethyl)trimethylsilane. The crystal structures of 3, 6 and 7 are reported. 1-Acyloxygermatranes 26 and 27 are obtained by treatment of 1-methoxygermatrane (28) with diphenyl- and dichloroacetic acid, respectively.
    Additional Material: 4 Ill.
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    Lithium 2,2,6,6-Tetramethylpiperidinoselenolate: An Unsymmetrical Dimer with an Unusually Coordinated Lithium (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 119-122 
    Details
    ISSN: 0009-2940
    Keywords: Selenolate ; Aminoselenolate ; Lithium compound i Ab initio calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Lithium 2,2,6,6-tetramethylpiperidide inserts elemental selenium into its Li-N bond with the formation of lithium 2,2,6,6-tetramethylpiperidinoselenolate 1. In the crystal 1 is an unsymmetric dimer. One lithium atom is coordinated tetrahedrally by two molecules of tetrahydrofuran and two selenium atoms, the other lithium atom exhibits an approximately rectangular-planar coordination by two N,Se-chelating groups. The lithium atoms are bridged by two selenium atoms thus forming a planar Li2Se2 core. Ab initio Hartree-Fock calculations show 1 and the hypothetical symmetric dimer 2 to be of equal energy, whereas the non-chelated dimer 3 is of distinctly higher energy. Exclusive crystallization of 1 is most likely a consequence of its large dipole moment of 6.18 D. Calculations also show that the deformation of the observed geometry around the uniquely coordinated lithium atom in 1 towards distorted tetrahedral or complete planarity leads to an increase of energy. Excessive charge transfer from selenium to nitrogen explains the overwhelming tendency for the N,Se-chelating bonding.
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    URL: http://dx.doi.org/10.1002/cber.19971300120
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    The Gas-Phase Structure of Trifluoromethyl Vinyl Sulfide, CF3SC(H)=CH2Dedicated to Prof. Dr. mult. Dr. h.c. Alois Haas on the occasion of his 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 131-134 
    Details
    ISSN: 0009-2940
    Keywords: Trifluoromethyl vinyl sulfide ; Gas-phase structure ; Electron diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The geometric structure of trifluoromethyl vinyl sulfide, CF3SC(H)=CH2, was determined by gas electron diffraction and ab initio calculations (HF/3-21G* and MP2/6-31G*). A single conformer with a dihedral angle φ(C=C-S-C) = 129(4)° is present. The conformational properties are compared to those of the parent compound, CH3SC(H)=CH2, and of the perfluorinated species CF3SC(F)=CF2.
    Additional Material: 3 Ill.
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    Bildung und Charakterisierung des Dinatrium-tetraphosphendiids (tBu3Si)NaP-P=P-PNa(SitBu3) und seines Dimeren (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 135-140 
    Details
    ISSN: 0009-2940
    Keywords: Synthesis ; Phosphorus ; Supersilyloligophosphides ; Crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of P4 in THF or DME with 2 R*Na (R* = SitBu3) at -78°C leads quantitatively to deep red THF or DME adducts of R*NaP-P=P-PNaR* (3). According to 31P NMR, the P4 skeleton 3 is cis-configurated. On the other hand, reaction of P4 in TBME with 2 R*Na at -78°C leads quantitatively to (R*NaP)4 (4), a [2+2] cycloadduct of 3, the Na4P8 skeleton of which according to X-ray structure analysis forms a double cube with four P atoms in the second layer and two P and two Na atoms in alternating positions in the first and in the third layer (the Na atoms are coordinated with donors). By resolving the THF adduct 3 in TBME (the TBME adduct of 4 in THF) the compound 4 (the compound 3) is rapidly formed under reversal of the P-P=P-P configuration by way of [2+2] cycloaddition (by way of [2+2] cycloreversion). 3 and 4 are sensitive to oxidation and to protolysis. With TCNE, 3 is oxidized to R*2P4 (bicyclic P4 skeleton), with CF3SO3H, 3 may be transformed into R*3P5Na2 X 4 THF or in (R*P3)3 and R*PH2.
    Additional Material: 4 Ill.
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    Recent Advances in C-F Bond Activation (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 145-154 
    Details
    ISSN: 0009-2940
    Keywords: Fluorocarbons ; C-F bond activation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The main reaction pathways which lead to the breaking of C-F bonds in perfluoroalkanes and -arenes are discussed. Emphasis is placed on recent developments and on the mechanistic patterns that emerge.
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    URL: http://dx.doi.org/10.1002/cber.19971300203
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    Matrix-Isolation of Iodine Superoxide and Iodine Dioxide (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 179-181 
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    ISSN: 0009-2940
    Keywords: Matrix isolation ; Pyrolysis ; Photochemistry ; Iodine compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Flash pyrolysis of a gas mixture containing iodine, oxygen and argon yields the hitherto unknown iodine superoxide, which can be identified by its UV absorption (λ max= 254 nm) after trapping the pyrolysate at 12 K. Irradiation converts iodine superoxide into iodine dioxide, identified by its IR and UV spectra.
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    URL: http://dx.doi.org/10.1002/cber.19971300207
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    Metal Atoms in the Synthesis of Metal Clusters, VIII.On the Reaction of Sterically Demanding Cyclopentadiene Ligands with Cobalt Atoms: Synthesis, Crystal Structure, Spectroscopic Behavior, and Reactivity of Di-, Tri- and Tetranuclear Hydrido Clusters of CobaltDedicated to Professor IV Siehert on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 161-170 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The metal-vapor reactions of Co atoms with 1,3-tBu2CpH (1a), 1,3-tBu2CpH (1a), 1,2,4-tBu3CpH (1b) and EtMe4CpH (1c) are described. With 1a the two mononuclear complexes [(η5-tBu2Cp) (η4-tBu2-1,3-cyclopentadiene)Co] (2a) and [(η5-tBu2Cp)2Co] (3a) were isolated, together with the dinuclear cobalt cluster [{(η5-tBu2Cp)Co}2H3] (4a) and trace amounts of the tetranuclear cluster [{(η5-tBu2Cp)CoH}4] (5a). The molecular structures of 3a and 4a were determined by X-ray diffraction. Reaction of 1b with Co atoms afforded a single product, the dinuclear cluster [{(η5-tBu3Cp)Co}2H3] (4b), whose molecular structure was determined by single-crystal X-ray diffraction. Both, 4a and 4b exhibit extremely short Co-Co distances [2.244(1) (4a) and 2.242(1) Å (4b)], as found for the Me5Cp analog [{(η5-Me5Cp)Co}2H3] (4c). Reaction of an isomeric mixture of Me4EtCpH (1c) with Co atoms furnished the mononuclear sandwich [ (η5-Me4EtCp)(η4-Me4Et-1,3- cyclopentadiene)Co] (2b), the trinuclear hydridocobalt cluster [{(η5-Me4EtCp)Co}3H4] (6a) and the tetranuclear hydridocobalt cluster [{(η5-Me4EtCp)Co}4H4] (5c). The molecular structure of 5c was determined by X-ray crystallography and revealed a tetrahedral arrangement of the cobalt atoms. The electrochemical behavior of the dinuclear complexes 4a-4c was studied by cyclic voltammetry. Reversible redox couples were found for all three compounds, with a correlation between the degree of alkyl substitution and their respective cathodic shifts. Compounds 4a and 4b react with CO to yield the mononuclear and dinuclear complexes [ (η5- CpR)Co(CO)2] (R=1,3-tBu2, 1,2,4-tBu3) (7a and 7b) as well as [{(η5-CpR)CO}2(CO)2] (8a and 8b). Reaction of the trinuclear hydridocobalt cluster 6a and its Me5Cp analog 6b with AgBF4 in the presence of PEt3 yielded the heteronuclear clusters [{η5-Me4CPR)Co}3AgP(Et)3H4]+[BF4]- (R=Et, Me) (9a and 9b). 9a was structurally characterized by X-ray crystallography.
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    Acetylene/Vinylidene Rearrangements of Fe(CO)2L2(silylacetylene) Complexes (L=Phosphorus Donor) (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 183-194 
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    ISSN: 0009-2940
    Keywords: Iron ; Alkyne complexes ; Vinylidene complexes ; C-H oxidative addition ; Rearrangements ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of a mixture of Fe(CO)2(PEt3)2N2 (1a) and [Fe-(CO)2(PEt3)2]2N2 (1b) with acetylene leads to three complexes: Fe(CO)2(PEt3)2(π-HC≡CH) (2a), Fe(CO)2(PEt3)2(H)(C≡CH) (2b), and Fe(CO)2(PEt3)2=C=CH2 (2c). Upon chromatography on silylated silica gel the mixture of 2a-c is completely transformed into 2c. The analogous reaction of 1a, b or of Fe(CO)2[P(OiPr)3]2N2 (1d) with HC≡CSiMe3 affords the primary oxidative addition products Fe(CO)2L2(H)(C≡CSiMe3) [L = PEt3, 3a; L = P(OiPr)3, 3c]. The presence of a small amount of Al2O3 in hexane irreversibly converts 3a and 3c into the vinylidene compounds Fe(CO)2L2=C=C(H)SiMe3[L = PEt3, 4a; L = P(OiPr)3, 4c]. The chromatographic work-up of 4c additionally leads to the hydrolysis product Fe(CO)2[P(OiPr3)2]2=C=CH2 (2d). The reaction of the phosphite-substituted derivative Fe(CO)2[P(OMe)3]2I- (1c) with silylacetylene allows detection of the acetylene species Fe(CO)2 [ P(OMe)3]2 (HC ≡CSiMe3) (3b), as well as the acetylido hydrido derivative Fe(CO)2[P(OMe)3]2(H)(C=CSiMe3) (4b). In a slow subsequent process, or with promotion by Al2O3 in hexane, the vinylidene compound Fe(CO)2[P(OMe)3]2=C=C(H)SiMe3 is formed. 3b or 4b are hydrolyzed to Fe(CO)2[P(OMe)3]2=C=CH2 (5c) in the presence of SiO2. The reaction of disilylacetylene with 1a-d results in the formation of disilylvinylidene complexes Fe(CO)2L2=C=C(SiMe3)2 (L = PMe3, 7a; L=PEt3, 7b; L = PiPr3, 7c). An intermediate acetylene derivative could be isolated for L = PEt3 (6a) and spectroscopically detected for L = P(OMe)3 (6b), but could not be traced for L = P(OiPr)3. Further studies were devoted to the reactions of silyl diynes (Me3SiC≡CR, R = C≡CSiMe3, p-C6H4-C-CSiMe3) with 1a-c. In all cases the acetylene compounds Fe(CO)2L2(Me3-SiC≡CR) [L = PEt3, R = C≡CSiMe3, 8a; R = p-C6H4-C≡CSiMe3, 9a; L = P(OMe)3 R = CSiMe3, 8b; R = p-C6H4-C≡CSiMe3, 9b] were isolated, but only for 8b was an equilibrium process observed to form the corresponding vinylidene derivative Fe(CO)2[P(OMe)3]2=C=C(SiMe3)C-C-SiMe3 (10b). 10b hydrolyzes upon chromatography on silica gel to give Fe(CO)2[P(OMe)3]2=C=CH-C≡CSiMe3 (11b): Finally, the reaction of p-diethynylbenzene with 1a-c was explored. The acetylido hydrido species Fe(CO)2L2(H)C≡C-p-C6H4-C≡CH was isolated in the case of L = PEt3 (12a) and spectroscopically detected for L = P(OMe)3 (12b). 12b and 12a transform spontaneously and in the presence of Al2O3 in hexane, respectively, to the vinylidene complexes Fe(CO)2L2=C=C(H)R [R = C6H4-C≡CH, L = PEt3, 13a; L = P(OMe)3, 13b]. 6a, 7a, and 8a have been characterized by single-crystal X-ray diffraction studies.
    Additional Material: 2 Ill.
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    Linked Benzylamido-Cyclopentadienyl Ligands: Synthesis and Characterization of Alkyl Titanium Complexes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 209-215 
    Details
    ISSN: 0009-2940
    Keywords: Titanium ; Amidocyclopentadienyl ligand ; Alkyltitanium compounds ; Lewis acids ; Agostic interactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Titanium complexes of the general type Ti(η5:η1-C5H4Si-Me2NCH2C6H3X2-2,5)Cl2 (X=H, F), containing a linked benzylamido-cyclopentadienyl ligand, were prepared by reaction of Ti(η5-C5H4SiMe2Cl)Cl3 with lithium amide Li(NHCH2C6H3X2-2,5). A single-crystal X-ray structural analysis of Ti(η5: η1-C5H4SiME2NCH2C6H3F2-2,5)Cl2 revealed a conformation in the solid state in which the aryl ring is turned away from the metal center. Ti(η5:η1-C5H4SiMe2NCH2C6H5)Cl2 can be alkylated with a variety of reagents to form extremely sensitive complexes of the type Ti(η5-C5H4SiMe,2NCH2C6H5)R2 (R=Me, CH2 C6H5, CH2SiME3, CH2CMe2C6H5). Reaction of Li2[C5Me4SiMe2NCH2C6H5] with TiCl3(THF)3 gave Ti(η5: η1-C5Me4SiMe2NCH2C6H5)Cl2, which can also be alkylated to form dialkyl complexes of the type Ti(η5:η1-C5Me4SiMe2NCH2C6H5)R2(R=Me, CH2C6H5, CH2SiMe3, C6H5).A single-crystal X-ray structural analysis of Ti(η5:η1-C5Me4SiMe2NCH2C6H5)(CH2C6H5)2 suggests the presence of α-agostic bonding of one of the titanium-bound CH2C6H5 groups to the titanium center.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300211
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    Masthead (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997) 
    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.19971300801
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  • 166
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    New Coupling Reactions and Phosphorylations Using Organozinc Reagents (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1021-1027 
    Details
    ISSN: 0009-2940
    Keywords: Zinc ; Chirality ; Cross-coupling ; Phosphorylations ; Catalysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This Microreview on the chemistry of organozinc reagents starts by briefly showing the methods of preparation of organozinc compounds and then discusses the considerable synthetic utility of zinc organometallics for the formation of new carbon-carbon bonds in the presence of transition-metal catalysts. Finally, the use of organozinc chemistry for the preparation of polyfunctional and chiral phosphanes is described.
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    URL: http://dx.doi.org/10.1002/cber.19971300802
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    Synthesis and Structures of Bis(tetramethylipiperidino)aluminum Halides-X-ray Crystal Structures of tmp2AlX (X = Cl, Br, I) and [tmp2A1(μ-F)l2 (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1047-1052 
    Details
    ISSN: 0009-2940
    Keywords: Bis(tetramethylipiperidino)aluminum halides ; Alkoxy((tetramethylpiperidino)aluminum halides ; 27Al-NMR spectra ; Aluminum ; Amides ; Synthetic methods ; Bridging ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: N-Lithio-2,2,6,6-tetramethylpiperidine [Li(tmp)] reacts with AlX3 (X = Cl, Br) in diethyl ether/ n-hexane solution to generate the products of substitution and ether cleavage, [tmpAl(X)(μ-OEt)], (la, X = Cl; 1b, X = Br). However, when the reaction is allowed to proceed in n-hexane alone, an almost quantitative yield of compounds tmp2AlX (2a, X = Cl; 2b, X = Br; 2c, X = I) is obtained. According to 27AI-NMR spectroscopy, mass spectroscopy, cryoscopy, and X-ray crystal structure determinations, these compounds are monomeric in the solid state, in solution, and in the gas phase. 2b reacts with AgBF4 yielding the fluoride-bridged dimer (tmp2AlF), 2d, as shown by X-ray crystal structure determination.
    Additional Material: 3 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19971300805
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  • 168
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    Synthesis, Structure, and Dynamic Behavior of (μ-Aldimido)(μ-η1: η2-alkyne)- biszirconocene Cation Complexes That Contain Planar-Tetracoordinate Carbon (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1069-1077 
    Details
    ISSN: 0009-2940
    Keywords: Planar-tetracoordinate carbon ; Dynamic organometallic systems, μ-alkyne complexes ; π-Agostic systems ; Zirconium ; Metallocenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The benzonitrile hydrozirconation product Cp2ZrCl(N—CHPh) 8 was treated with propynyl lithium to yield the (propynyl)(benzaldimido)ZrCp; complex 9. Subsequent treatment with trityl tetraphenylborate generated [Cp2Zr(C—C—CH3)-BPh-4] that instantaneously added to 9 to eventually form the (μ-aldimido)(μ-η1:η2-hexadiyne)ZrCp2 cation 11. The X-ray crystal structure analysis showed that 11 contains a planar-tetracoordinate carbon atom that is stabilized by forming a three-center-two-electron bond with the two adjacent metal atoms. Similarly, complex 9 reacted with [Cp2Zr(CH3)+CH3B(C6F5)3 1 to yield the planar-tetracoordinate carbon containing (μ-aldimido)(μ-η1:η2-2-butyne) Cp; cation 12. Both complexes 11 and 12 exhibit dynamic NMR spectra due to their rapid reorganization of the dimetallabicyclic frameworks (ΔG* = 10 kcal mol-1) in addition to an anchimerically assisted C—N bond rotation (ΔG* =15 kcal mol-1).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300808
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    On the Oxenoid Character of Alkylperoxy Anions and Their Lithium Compounds: A Combined Mass-Spectrometric and Theoretical Investigation (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1085-1097 
    Details
    ISSN: 0009-2940
    Keywords: Mass spectrometry ; Peroxides ; Oxenoids ; Density functional theory ; Kinetic energy release ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A combined mass-spectrometric and theoretical approach has been used for an investigation of the gas-phase chemistry of two representative alkylperoxy anions. Metastable CH3OO- ions undergo unimolecular loss of molecular hydrogen and formaldehyde yielding HCO-2 and OH-, respectively. The observed reactivity is in pleasing agreement with calculations of the [C,H3,O2- and [C,H,O2]- potential-energy surfaces at the BECKE3LYP/6-311+ + G** level of theory. Upon exhaustive methylation of the α-position as in t-C4H9OO- anions, the reactivity switches completely to an elimination of (CH3)2C=CH2 giving rise to the formation of HOO-. The results obtained for the “bare” alkylperoxy anions are used for the analysis of the EI mass spectrum of (t-C4H9OOLi)12 dodecamers, which thermally decompose in the inlet system at a probe temperature of ca. 130°C. The decomposition is rationalized by a mechanism involving nucleophilic attack of one t-C4H9OOLi subunit on the oxenoid oxygen atom of a second t-C4H9OOOLi moiety. This reaction may produce t-C4H9OOOLi trioxy species as intermediates, which rapidly decompose to singlet dioxygen and t-C4H9OLi.
    Additional Material: 4 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19971300810
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    Thio-Ligation to Vanadium: The NSSN and S′N′O Donor Sets (N = Pyridine, N′ = Enamine; S = Thioether, S′ = Thiolate) (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1129-1133 
    Details
    ISSN: 0009-2940
    Keywords: Vanadium ; S Ligands ; Schiff bases ; N ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tetradentate, neutral disulfide [bis(thioether)] ligand 1,6-bis(o-pyridyl)-2,4-dithiahexane, NSSN, reacts with [VCI2(tmeda)2] to form the octahedral (all-cis; C2v-symmetric) complex [VCl2(NSSN)] 1, the first low-valent vanadium complex in which the thio functions are exclusively organic sulfides. Treatment of (VOCl2(thf)2] with O-mercaptoaniline, followed by reaction with o-hydroxynaphthaldehyde yields the non-oxo V′” complex [V(S′N′O)2] 2, derived from the Schiff base HS′N′OH, where 0 and S′ are phenolate and thiophenolate functions, respectively, and N′ is the Schiff base (enamine) nitrogen. Complex 2, with the ligands in a distorted trigonal-antiprismatic array, is a rare example of a structurally characterized complex where the Schiff base is preserved at the expense of its thiazoline tautomeric form.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300815
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    Contributions of the Chemistry of Boron, 236. In Quest of New and Stable Bis(organyloxy)boranes (RO)2BH for Catalytic HydroborationDedicated to Prof. Dr. Marianne Baudler on the occasion of her 75th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 363-370 
    Details
    ISSN: 0009-2940
    Keywords: Bis(triphenylmethoxy)hydroborane ; Naphtho[2,3-d], -1,3,2-dioxaborolane ; Naphtho[1,8-de]-1,3,2-dioxaborinane ; Phenanthro[9,10-d]-1,3,2-dioxaborolane ; Dibenzol[d,g]-1,3,2-dioxaborocine ; Bis(diphenylmethoxy)borane ; Tetrachlorobenzo-1,3,2-dioxaboraolen ; Hydroborations ; Boron ; Catalysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New and stable bis(organyloxy)boranes, 1,3,2-dioxaborolanes and 1,3,2-dixoaborinanes have been prepared (i) from the corresponding diol and BH3·THF and (ii) from 1,2-diketones and BH3·THF. They were characterized by spectroscopic techniques. The BH stretching frequency seems to be a measure of ring strain and Lewis acidity. The compounds have been qualitatively tested in the transition-metal-catalysed hydroboration of cyclopentene, and the dioxaborinane 11 proved to be superior to the 1,3,2-dioxaborolanes 9 and 18.
    Additional Material: 2 Ill.
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    A New Efficient Synthesis of the Stilbenoid Laser Dyes BPS and Stilbene I by Palladium-Catalyzed Coupling of Ethene with Bromoarenes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1193-1195 
    Details
    ISSN: 0009-2940
    Keywords: Stilbene ; 4.4′-Diarylstilbenes ; Palladium ; Pd-catalyzed ; C-C coupling ; Dyes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The palladium-catalyzed coupling of ethene with 4-bromobiphenyl and 4′-bromo-4-biphenylsulfonic acid permits a facile one-pot preparation of the laser dyes (E)-4,4′-diphenylstilbene (BPS, 3) and bis(triethylammonium) (E)-4,4′diphenylstilbene-4″,4″-disulfonate (6) in diastereomerically pure form on a multigram scale, with yields of 69 and 64%, repectively. The latter can easily be transformed to its dipotassium salt 7, the Stilbene I dye.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19971300905
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    Synthesis and Properties of Me2Ge-Bridged Arenes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 421-424 
    Details
    ISSN: 0009-2940
    Keywords: Macrocycles ; Germanium ; UV/Vis spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Linear and cyclic oligomers of Me2Ge-bridged π-systems have been obtained by the reaction of carbo- and heterocyclic anions and dianions with Me2GeCl2. The spectroscopic properties of the new compounds are compared with analogous carbon- and Me2Si-bridged π-systems.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19971300318
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    Organoamido- and Aryloxolanthanoids, 15Part 14: Ref. [1a].. Organometallic Compounds of the Lanthanoids, 116Part 115: Ref. [1b].. Syntheses of Low Coordination Number Divalent Lanthanoid Organoamide Complexes, and the X-ray Crystal Structures of Bis[(N-2,6-diisopropylphenyl)(N-trimethylsilyl)amido]bi(tetrahydrofuran)samarium(II)and -ytterbium(II) (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 409-415 
    Details
    ISSN: 0009-2940
    Keywords: Mercury ; Lanthanides ; Lanthanoid(II) complexes ; (N-2,6-Diisopropylphenyl)(N-trimethylsily)amide complexes ; Bis(trimethylsilyl)amide complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Mercury(II) amide complex Hg[N(SiMe3)(2,6-iPr2C6H3)]2 (1) was prepared by reaction of HgBr2 with Li[N(SiMe3) 2,6-iPr2C6H3)] in diethyl ether solvent. Redox transmetallation reactions of 1 with elemental samarium, europium or ytterbium in THF solvent (THF = tetrahydrofuran), generated the novel divalent complexes Ln[N(SiMe3)(2,6-iPr2C6H3]2(THF)2 with Ln = Sm (2), Eu (3) and Yb (4). 4 was also synthesized by reaction of elemental ytterbium, HgPh2 and HN(SiMe3)(2,6-Me3)2]2(THF)2 [Ln = Sm (5), Yb (6)] by reaction of the metals with HgPh2 and HN(SiMe3)2. Thermal desolvation of 4 under high vacuum gave Yb(N)(SiMe3)2,6-iPr2C6H3)]2 (THF) (7), whereas under identical conditions 6 yielded the solvent-free complex [Yb[N{SiMe3)2]2]2. (8). The new compounds 1-4 and 7 are hydrocarbon soluble and 171Yb-NMR spectra were recorded for 4, 6, 7 and 8. X-ray crystal structure determinations of 2 and 4 revealed four-coordinate, distorted tetrahedral metal environments augmented by weak Ln…ipso-C(aryl) interactions.
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    URL: http://dx.doi.org/10.1002/cber.19971300316
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    Unsymmetric Dinucleating Ligands for Metallobiosite Modelling (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 433-442 
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    ISSN: 0009-2940
    Keywords: Metallobiosites ; Metalloproteins ; Metalloenzymes ; Dinucleating ligands ; Transition metals ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Awareness of the asymmetric nature of numerous dinuclear metallobiosites and of the ability of the individual metal ions to have quite distinct roles in the functioning of the metalloenzyme concerned has led to a search for carefully designed unsymmetric dinucleating ligands that will give dinuclear complexes capable of acting as models for the metallobiosites. This review surveys progress made in the design and synthesis of complexes capable of serving as models for donor atom, coordination number and geometric asymmetries found at dinuclear metal centres.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300402
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    The Equilibrium Between 2-Lithium-Oxazole(-Thiazole, -Imidazole) Derivatives and Their Acyclic Isomers - A Structural InvestigationDedicated to Professor Dr. D. Seebach on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1213-1221 
    Details
    ISSN: 0009-2940
    Keywords: 2-Li(ZnCl)-substituted oxazoles (thiazoles, imidazoles) ; Acyclic isomers ; NMR spectroscopy ; Lithium ; Zinc ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 2-Metallated oxazoles, thiazoles and imidazoles are of interest for the preparation of derivatives of the respective heterocycles, and - especially in the case of metallated thiazoles - as acyllithium equivalents in organic syntheses. Metallation at C2 of these compounds, however, often leads (more so with Li-oxazoles than with Li-thiazoles and Li-imidazoles) to products derived from the acyclic isomers of the metallated heterocycles. In order to obtain more information on the positions of the relevant equilibria, we have carried out a 13C-NMR study of substituted li- and ZnCl-oxazoles, Li-thiazoles and Li-imidazoles. In the case of Li-oxazoles, the equilibrium is completely on the side of the acyclic isomers. Addition of ZnCl2, however, leads to ring-closure, and, even in the case of 2-ZnCl-substituted benzoxazole, only the ring-closed isomer is observed. This demonstrates a dramatic gegenion effect on the equilibrium between two isomeric anions. In the case of Li-thiazoles, depending on the substitution pattern, either solely the ring-closed or an equilibrium with the ringopened isomer is observed. In the series of Li-imidazoles, only the 2-lithiated benzimidazole is in equilibrium with its ring-opened isomer. The tendency of these compounds to undergo ring-opening parallels the leaving group properties of the various subunits [OLi 〉 SLi 〉 R2NLi, and phenyl-O(S, NR)Li 〉 vinyl-O(S, NR)Li]. The difference between the effects of Li+ vs. ZnCl+ in the (benz)oxazole series is in agreement with results of solid-state structure investigations of 2-lithiated and a 2-zincated thiazole: in the Li compound the C-S bond is 2.9 pm longer than in the ZnCl species, indicating a more facile C-S bond cleavage with Li+ as the gegenion.
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    URL: http://dx.doi.org/10.1002/cber.19971300908
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    Synthesis, Redox Chemistry, and Mixed-Valence Phenomena of Cyanide-Bridged Dinuclear Organometallic Complexes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1241-1252 
    Details
    ISSN: 0009-2940
    Keywords: Organometallic complexes ; Cyanide bridges ; Structure elucidation ; Isomerizations ; Oxidation ; Mixed valent compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 21 new organometallic complexes of the type M-Cn-M′ containing the building blocks M, M′ = (CO)5Cr, (CO)5Mo, (CO)5W, Cp(CO)2Mn, Cp(CO)2Fe, Cp(CO)(CN)Fe, Cp(dppe)Fe, Cp(PPh3)2Ru, Cp(PPh3)Ni, and (PPh3)2Ag were obtained from the reagents M-Cn and M-X (X = leaving group). Among them are five pairs of linkage isomers M-CN-M′/M-NC-M′. Structure determinations of (CO)5Cr-CN-M′ with M′ = Fe(dppe)Cp, Ni(PPh3)Cp, Ag(PPh3)2 and of (CO)5Cr-NC-Fe(dppe)Cp have proved their identity and the linkage isomerism. Systematic variations of the v(CN) and v(CO) IR bands allow as assessment of the relative electron pair acceptor strengths of the building blocks M and M′ and a reliable identification of the individual linkage isomers. All dinuclear complexes are redox-active, showing at lease one reversible oxidation. The redox potentials are characteristically dependent upon the nature of the building blocks M and M′ and upon the orientation of the cyanide link (CN vs. NC), 6 oxidized complexes of the type [M-Cn-Fe(dppe)Cp]+ were prepared chemically and isolated as PF6 or BF4salts. The molecular structure of [(CO)5Cr-CN-Fe(dppe)Cp]BF4 is not significantly different from those of the corresponding neutral Cr-CN-Fe or Cr-NC-Fe complexes. Upon oxidation the v(CN) band of the complexes shifts to lower wavenumbers and becomes much more intense. The oxidized complexes show the paramagnetism due to one unpaired electron. They give rise to very intense metal-to metal charge-transfer bands in the near infrared region whose position was found to be characteristically dependent on solvent polarity of [(CO)5Cr-CN-Fe(dppe)Cp]BF4. A semiquantitative treatment of the optical and electrochemical measurements shows that the electron delocalization and metal-metal interaction in the oxidized dinuclear complexes is significant and that they belong to the class-II mixed-valence systems.
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    URL: http://dx.doi.org/10.1002/cber.19971300912
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    Benzil Derivatives as Trapping Reagents for the Monomeric Alkylindium(i) Compound in-c(SiMe3)3 (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1269-1272 
    Details
    ISSN: 0009-2940
    Keywords: Indium ; Clusters ; Low-valent compounds ; Trapping reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tetrahedral cluster compound tetrakis[[Tris(trimethylsilyl)methyl]indium(I)] 91) reacts in boiling n-hexane with benzil derivatives (p-X-C6H4)C(O)(p-X-C6H4) (X = H, OMe, Br), to yield the 1,4-cycloadditon products of the monomeric alkylindium(I), In-C(SiMe3)3, in which the In atoms are coordinated by a chelating enediolato ligand, to form a five-membered InO2C2 heterocycle. As shown by two crystal structure determinations (X = H, OMe), the products are dimeric in the solid state, with a four-membered In2O2 heterocycle in the molecular center and both C(SiMe3)3 groups, as well as both enediolato substitutents in a cis arrangement.
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    URL: http://dx.doi.org/10.1002/cber.19971300915
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    Tripod Ligands Containing a Mixed P/N/S Doner Set: Synthesis and Coordination Chemistry (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1279-1294 
    Details
    ISSN: 0009-2940
    Keywords: Tripodal ligands ; Aminolytic cleavage of oxetanes ; Tripod molybdenum compounds ; Mixed donor set ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation of neopentane-based tripod ligands CH3C(CH2X)(CH2Y)(CH2Z( 3 (X = NR2, NHR; Y = PR2; Z = PR2, SR, S-) in a convergent manner is described. The procedure is based on the aminolytic cleavage of functionalized oxetanes CH3C(CH2OCH2)CH2R 1 by primary or secondary amines, leading to functionalized amino alcohols CH3C(CH2NHR)(CH2OH)(CH2R) or CH3C(CH2NR2)-(CH2OH)(CH2R) 2. The appropriate activation of the R (e.g. OR) and OH groups present in 2 allows for substitution vs. SR or PR2 donor functions. Depending on the nature of the groups present in each reaction step, various protection and groups present in each reaction step, various protection and deprotection steps have to be taken in the course of this type of preparation of the tripod ligands 3. By reaction with (CH3CN)3Mo(CO)3, ligands 3 form Mo(CO)4 derivatives 4 or Mo(CO)3 derivatives 5, depending on the reaction conditions. In compounds 4, the ligands are coordinated in a bidentate mode with the soft donor atoms (P, S) coordinated and the hard donor function playing the role of the dangling arm. In the trihapto bonding mode present in 5, all three donor functions, two soft (P, S) and one hard (NHR′, NR′2), are coordinated. The two types of coordination compounds may be interconverted: 4e (X = NMe2′ Y = PPh2, Z = SiPr) with a non-coordinating CH2NMe2 group is transformed into 5c upon photolytic decarbonylation. Under 1 bar CO at 20°C, 5c reverts to 4e. X-ray structure analysis of a series of compounds of types 4 and 5 reveals characteristics of the relevant conformational patterns. All compounds have been fully characterized by the standard analytical techniques (NMR, MS), as well as elemental analysis.
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    Dinuclear Cobalt(II) Complexes of Pyrazole Ligands with Chelating Side ArmsDedicated to Prof. Dr. Walter Siebert on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 605-613 
    Details
    ISSN: 0009-2940
    Keywords: Pyrazolate complexes ; Dinuclear complexes ; Bridging ligands ; Cobalt ; Conformational analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of pyrazole-based potential ligands bearing polydentate amine substituents in the 3- and 5-positions of the heterocycle has been synthesized [3,5-bis(R2NCH2)-pyzH R2N = Me2N(CH2)3NMe (2aH), [Me2N(CH2)3]2N (2bH), (Et2NCH2CH2)2N (2cH)]. Upon reaction with two equivalents of CoCl2 they form complexes LCo2Cl3 (3a-c; L = 2a-c, respectively) which are shown crystallographically to contain a dinuclear metal core bridged by both the pyrazolate unit and a chlorine atom, with each cobalt center carrying a further terminal chlorine atom. Two of the ligand side arms in 3b, c are dangling, thus leading to five-coordination of the cobalt(II) centers in all cases. Addition of two equivalents of NaBPh4 to solutions of 3b, c induced coordination of the formerly dangling side arms to the metal centers by substitution of the terminal chlorine atoms. The resulting compounds [LCo2Cl](BPh4)2 (4b, c, respectively) were characterized by X-ray structure analyses. They can be viewed as dinuclear linked versions of tran-type complexes [(tran = tris(aminoalkyl)amine] with distorted trigonal-bipyramidal coordination spheres around cobalt(II). Conformational analyses employing force-field calculations were carried out for 4b, c in order to rationalize the conformations observed in the solid state with regard to the accessible conformational space.
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    P/O Ligand Systems: Facile Synthesis, Structure, and Catalytic Tests of 2′-Phosphanyl-1,1′ -phenyl-2-ols and 2′-Phosphanyl-1,1′-binaphthyl-2-ols (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1663-1670 
    Details
    ISSN: 0009-2940
    Keywords: Lithiation ; P ligands ; NMR spectroscopy ; Molecular structure ; Hydrogenations ; Hydroformylations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A facile synthesis of 2′-phosphanyl-1,1′-biphenyl- and 2′-phosphanyl-1,1′ -binaphthyl-2-ols and their silyl ethers has been developed, consisting of electron-transfer-catalyzed ring-opening of dibenzofuran and dinaphthofuran, respectively, subsequent reaction with chlorophosphanes, and work-up with acetic acid or ClSiMe3. Studies of the molecular and crystal structures reveals the presence of P - H - O bridging bonds in the more basic tBuPhP derivative and a nearly perpendicular arrangement of the aryl planes in the biphenyl derivatives. The barrier to rotation of the aryl planes about the C-C axis was determined by NMR in the case of the P-asymmetric derivative 3d, using the appearence of diastereoisomers by atropisomerism and P-asymmetry. Comparative screening tests of the title compounds, phosphanyl phenols and phosphanylnaphthols in homogeneous Rh-catalyzed reactions demonstrate catalytic activity in hydroformylation reactions and superior properties of the biphenyl- and binaphthyl-2-ol derivatives in relation to other P-O ligands.
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    URL: http://dx.doi.org/10.1002/cber.19971301118
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    On the Polymorphism of White PhosphorusDedicated to Professor Gottfried Huttner on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1235-1240 
    Details
    ISSN: 0009-2940
    Keywords: Phosphorus ; Phase transitions ; Molecular crystal ; Crystal growth ; Low-temperature crystal structure ; Librational motion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: White phosphorus occurs in three modifications. The α form, which exists at roomtemperature, transforms reversibly to the β form at -77°C. The α · β transformation may be strongly delayed. Quenching the α form to -185°C followed by slow warming results in an exothermic reactions with formation of the γ form which transforms into the β form at -120°C in an endothermic reaction. A transition β · γ is not observed. The γ form is characterized by its powder diagram. The structure of the β form is redetermined from a single crystal at -185°C (P., α = 547.88(5), b = 1078.62(11), c = 1096.16(11)pm, α= 94.285(8), β = 99.695(7), γ = 100.680(7)., V = 623.79(10) · 106 pm3, Z = 6 formula units per cell). The P4 molecules exhibit pronounced librational motion in spite of the low temperature of investigation. The arrangement of the centers of the tetrahedra corresponds to the atom positions in the γ-plutonium structure, which is discussed in relation to the bcc structure.
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    Evidence for Internal Ion Pair Formation upon Insertion of Reactive Alkene in the Zirconium-Carbon Bond of the cp2Zr(μ-C4h6)b(c6f5)3 Metallocene-Boron-Betaine Ziegler Catalyst System (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1261-1267 
    Details
    ISSN: 0009-2940
    Keywords: Single-component metallocene catalyst ; Olefin insertion ; Organometallic ions pairs ; (Alkene)metallocene complex ; Metallocene betaines ; C-C coupling ; Zirconium ; Homogeneous catalysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of the (butadiene)ML2 complexes 1 [ML2 = Cp2Zr (a), Cp2Hf (b), and (.-C5H4CH3)2Zr (c)] with B(C6F5)3 gives the 1:1 addition products (CH2CHCHCH2-B(C6F5_3)ML2 (3a-c). At -40°C the betaine complex 3a inserts one equivalent of methylenecyclopropane to give the regioisomeric insertion products 5a and 6a in a 60:40 ratio. These products exhibit the cyclopropylidene moiety in the α- and β-positions, respectively, relative to zirconium. The corresponding hafnocene complexes 5b and 6b are obtained in a 70:30 ratio starting from 3b. The reaction of 3(a-c) with allene gives a single insertion product (7a-c) in each case where the exo-methylene group is in the α-position to the metal center ([2,1]-insertion). The complexes 5-7 are chiral. They all exhibit a pronounced ·-interaction of the internal -C4H=C5H- double bond of the s̰-ligand chain with the metal center in addition to a metallocene/-C6H2-[B] ion pair interaction. The relative contributions of the cationic metallocene end of the dipolar complexes 5-7 are quite dependent on the steric and electronic properties of the respective metallocene units involved. This is revealed by a comparison to typical 13C-NMR parameters of the complexes 5-7 with a pair of suitable model complexes, namely the ethylene insertion product 4 into the betaine system 3a and its THF adduct 4.THF.
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    New Borylene Complexes of the Type [μ-BX{.5-C5H4Me)MN(CO)2}2]: Substitution Reactions at the Metal-Coordinated Borylene Moiety (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1295-1298 
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    ISSN: 0009-2940
    Keywords: Boron ; Manganese ; Borylene complexes ; Reactions at metal-coordinated boron ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of the air- and water-stable borylene complex [μ-BNMe2{.5-C5H4Me)Mn(CO)2}2] (1a) with a solution of Hcl in Et2O affords the correspondin chloroborylene complex [μ-Chloroborylenebis{dicarbonyl(.5-methylcyclopentadienyl)manganese}(Mn-Mn)] (2). This compound easily undergoes further substitution reactions with protic reagents such as primary amines, alcohols and water at the metal coordinated borylene moiety with elimination of HCl, giving new products of the type [μ-BX{.4-C5H4ME)Mn(CO)2}2] (3a, ab: X=NHtBu, NHPh; 4a, b: × = OMe, OEt; 5: X= Oh}. All borylene complexes were isolated as crystalline solids in good yield and characterized by multinuclear NMR methods and IR spectroscopy in solution. In addition, the structure of 4b in the crystalline state was determined by a single-crystal X-ray study.
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    Halogenation of 1-Ethoxy-1-oxophosphindolin-3-one, a Potential Phosphaindigo Precursor (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1765-1770 
    Details
    ISSN: 0009-2940
    Keywords: Phosphinic acid ; Phosphaindole bromination and chlorination ; Layer structure ; Hydrogen bonds ; Bromine-bromine interaction ; Phosphorus heterocycles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The bromination of 1-ethoxy-1-oxophosphindolin-3-one (1) with two equivalents oi bromine occurs with elimination of hydrogen bromide and ethyl bromide, providing 2,2-di- bromo-1-hydroxy-1-oxophosphindolin-3-one (4) in high yield. In the presence of triethylamine this process leads to 2,2-dibromo-1-ethoxy-1-Oxophosphindolin-3-one (3) instead. Triethylamine deprotonates 4, providing the solid triethylammonium salt 5. Silylation of 4 with chlorotrimethylsilane leads to the trimethylsilyl ester 6. Monobromination in a two-phase reaction allows the isolation of a mixture of isomers of 2-bromo-1-ethoxy-1-oxophosphindolin-3-one (2a, b). Chlorination with chlorine furnishes 2,2-dichloro-1-ethoxy-1-oxo-phosphindolin-3-one (7). The new compounds 2-7 were characterized analytically and spectroscopically (EI-MS, 1H, 13C and 31P NMR). The crystal structure of acid 4 was determined by X-ray diffraction. Solid 4 consists of aryl stacks connected by chains of P—OH…O==P hydrogen bonds and secondary Br…Br contacts.
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    URL: http://dx.doi.org/10.1002/cber.19971301210
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    Synthesis of the Diazadisilatitanacyclopentane RSi(NH2)NHTiMe(cp*)NHSi(NH2)R (R =PhNSiMe3, cp *=η5-C5Me5 (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1787-1790 
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    ISSN: 0009-2940
    Keywords: Silicon ; Titanium ; Diazadisilatitanacyclopentane ; Aminodisilanes ; Tetrachlorodisilanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of two equivalents of N-trimethylsilylaniline (1) with two equivalents of n-butyllithium, followed by subsequent treatment with Si2Cl6 (2) leads to the formation of the tetrachlorodisilane RSiCl2SiCl2R (3) (R = PhNSiMe3). 3 is converted to RSi(NH2)2Si(NH2)2R (4) by reaction with liquid ammonia. 4 reacts with cp*TiMe3 (5) (cp* = η5-CsMe5) to yield the diazadisilatitanacyclopentane RSi(NH2)NHTiMe(cp*)NHSi(NH2)R (6). The crystal structure of 6 is reported.
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    A Novel Stoichiometry for Chlorogold(I) Complexes: Structure of L4Au3Cl3(L =pyrrolidine) (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1813-1814 
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    ISSN: 0009-2940
    Keywords: Amines ; Gold(I) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction between (tht)AuCl (tht = tetrahydrothiophene) and neat pyrrolidine (L) leads to the compound L4Au3Cl3. An X-ray structure determination reveals the presence of molecules LAuCl and ions L2Au+ and Cl-, in the ratio 2:1:1. The packing is characterised by Au.Au contacts and N-H-Cl-hydrogen bonds.
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    Kinetics and Mechanism of Substitution Reactions of cis-[PtMe2(dmso)2] with Pyridine (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1791-1799 
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    ISSN: 0009-2940
    Keywords: Platinum substitution ; Metal-carbon bonds ; trans-Labilization ; Kinetics ; Activation parameters ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The substitution reactions of cis-[PtMe,(dmso),] with pyridine (py) to produce cis-[PtMe2py2] in toluene proceeds in two steps. In the absence of added dimethylsulfoxide (dmso), these steps can not be separated due to the rate constants being very similar. In the presence of added dmso, the rate of the first step, the formation of the monopyridine complex is retarded, which is indicative of a dissociative mechanism. A parallel associative reaction path with pyridine could also be observed. This pathway is independent of the concentration of added dmso. Above a 40-fold excess of dmso, the dissociative pathway is suppressed and only the associative reaction occurs. A plot of Kobs vs the pyridine concentration for this pathway is linear at low [py], but shows a saturation at high [py]. This suggests that the reaction occurs via the formation of a precursor-complex, for which the formation constant was found to be 0.32 · 0.03 M-1. The volume of activation at a high pyridine concentration is -11.4 · 0.8 cm3 mol-1, which indicates that the ligand interchange process is of the associative type. The second step, the formation of the bispyridine complex, can clearly be separated from the first reaction step. This step occurs via a dissociative mechanism, as demonstrated by the decrease in kobs with increasing pyridine concentration. The dissociation of dmso was characterized by a rate constant of (8.1 · 0.9).10-45-1 at 25°C, ·H = 116 ·9 kJ mol-1 and AS. = 86 · 29 JK-1 mol-1. At higher pyridine concentrations evidence for a parallel associative reaction was found, for which the rate constant is (1.3 · 0.2).10-3 M-1S-1 25°C. The results are discussed in reference to available literature data.
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    Regioselective Complexation of New Multiple Piperazine/Pyridine Ligands: Differentiation by 113Cd-NMR Spectroscopy (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1353-1359 
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    ISSN: 0009-2940
    Keywords: 113Cd NMR ; Multidentate ligand ; Multinuclear metal complex ; Piperazine ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Eleven novel piperazine containing open-chain ligands L1-L11 were designed to offer symmetrical and asymmetrical complexation sites for metal ions and were synthesized by repetitive synthetic method. The divergent use of aromatic bishalomethyl and mono-N-alkylated piperazine compounds as spaces led toa series of long (up to M. W. = 836) oligomeric multidentate N-ligands. Due to the lack of solid state methods for structure analysis, an NMR technique using 113 Cd nucleus as a probe in solution state was utilised. 113 Cd chemical shifts were observed to be dependend on the coordination site and similar coordination sites in different ligands gave characteristically similar 113 Cd chemical shifts. As a result 113 Cd-NMR spectroscopy proved to be an excellent tool to distinguish between the structures of the different complexation sites on a nearly quantitative level.
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    Synthesis and Electrochemistry of Diels-Alder Adducts of [60] Fullerene with a Phthalocyanine and a Hemiporphyrazine (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1375-1378 
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    ISSN: 0009-2940
    Keywords: Phthalocyanines ; Hemiporphyrazines ; Fullerenes ; Diels-Alder reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of a new Diels-Alder adduct 7 of [60]fullerene and a phthalocyaninenickel compound containing a longer spacer than the originally reported Diels-Alder adduct 1 is described. The bisenophilic hemiporphyrazinenickel compound 11 reacts with [60]fullerene to form a Diels-Alder adduct 12 containing two fullerene units. Spectroelectrochemical investigations of 7 and 12 reveal multiple reductions, which are attributed to the corresponding subunits of the molecules. In contrast to 1, the election acceptor properties of the [60]fullerene unit in both molecules have no influence on the electronic properties of the phthalocyanine and hemiporphyrazine, respectively.
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    Diastereoselectivity in the Reaction of RCH2C[CH2P (Ar)(Lr)]3 with Electrophiles: Enhancement of Diastereoselective Control by η3-Coordination in {RCH2C[CH2P(Ar)(Li)3}Mo(Co)3 (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1379-1392 
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    ISSN: 0009-2940
    Keywords: Chiral tripod ligands ; Tripod Mo(CO)3 compounds ; Diastereoselective synthesis ; Separation of diastereomers ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Following a procedure developed for H3CC[CH2P(Ph)2]3 (1a) as the starting compound, various tripod ligands RCH2C[CH2P(Ar)2]3 (1) have been transformed into the trilithiotriphosphides RCH2C[CH2P(Ar)(Li)]3 with various electrophiles R′  -  Hal leads to the two diastereomers of RCH2C[CH2P-(Ar)(R)]3 (6) with an (RRR/SSS : RRS/SSR) ratio close to the statistical value of 1:3, except when Ar=Ph and R′=Bzl, where the RRS/SSR diastereomer is obtained almost exclusively. In contrast, the reaction of [RCH2C[CH2P(Ar)(Li)[3]-Mo(CO)3 (4) with electrophiles R′  -  Hal tends to favour the formation of the homochiral RRR/SSS diastereomers. The triphosphide coordination compounds 4 are available by two different routes: either the complexes (RCH2C[CH2P-(Ar)(H)]3Mo(CO)3, obtained from 2 and (CH3CN)3Mo(CO)3, are deprotonated by MeLi, or the trilithiotriphosphides RCH2C[CH2P(Ar)(Li)]3 are reacted with (CH3CN)3Mo(CO)3 to produce 4 in high yields. The ration in which the two diastereomeric forms of 5 are obtained depends on the nature of the electrophile: the greatest diastereomeric discrimination is obtained for Ar=Ph, R=Ph, R′=Bzl, where the homochiral relative to the RRS/SSR pair. Two-dimensional NMR spectra and simulations of one-dimensional spectra are used to ascertain the diastereomeric excess in each case. X-ray analyses of three compounds of type 5 (5d, Ar=Ph, R=H, R′=Ph, R′=Bzl) indicate the remarkable conformational stability of the tripod metal scaffolding, with the conformations observed for these three compounds in three different solid-state environments being closely similar, even with respect to the torsional arrangement of the phosphorus-bound benzyl groups.
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    Tetramethylguanidine and Benzophenoneimine as Ligands in Gold Chemistry (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1417-1422 
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    ISSN: 0009-2940
    Keywords: Gold ; N ligands ; Gold(I) complexes ; (Imine)gold(I) complexes ; Guanidines ; Ketimines ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (Tetramethylguanidine)gold(I) chloride (1) and bromide (2) are readily prepared in high yield from (Me2N)2C=NH and [AuCl(Me2S)] or [AuBr(tht) (tht = tetrahydrothiophene), repectively. NMR spectra of chloroform solutions of the two products indicate equilibria of the type 2 LAuX = L2Au+AuX2-. The cationic complex [Au(NH=C(NMe2)2)(PPh3)]+ is obtained as the triflate salt 3 from tetramethylguanidine and [Au(PPh3)]+O3SCF3-. In solution at low temperature (-60°C), this compound adopts a rigid structure whereby the NMe2 groups are rendered non-equivalent, but at ambient temperature there is coalescence of the NMe2 signals in the 1H- and 13C-NMR spectra. The related benzophenoneimine complex [Au{NH=CPh2}(PPh3)]+BF4- (4), which was synthesized as a reference3 compound, exhibits similar behaviour. In solution at low temperature (-60°C) the two phenyl rings of the ligand are diastereotopic. In contrast, the triisopropylphosphane derivative [Au[NH=CPh2](PiPr3)]+BF4- (5) is rigid on the NMR time scale, even at 25°C. Thbe solid-state structures of 2, 3, 4, and 5 have been determined by single-crystal X-ray diffraction. Compound 2 crystallizes in the ionic form with discrete Au … Au bonded ion pairs [Au[NH=C(NMe2)2]2]+ [AuBr2]- [Au … Au 3.1413(8) Å]. The cations of 3, 4, and 5 show the [Au(PPh3)]+ units N-coordinated to the imino groups, with the nitrogen atoms in a trigonal-planar configuration.
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    URL: http://dx.doi.org/10.1002/cber.19971301010
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    Olefin Carbonylation Catalysis with Cationic Palladium Complexes: Selectivity and Possible Intermediates (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1557-1565 
    Details
    ISSN: 0009-2940
    Keywords: Carbonylations ; Alkenes ; Palladium ; Asymmetric catalysis ; P and N ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Palladium complexes L2PdX2 containing various group Va ligands and weakly coordinating anions are active catalysts for the carbonylation of olefin substrates. These catalytic systems, though gaining significance in industry for the synthesis of polyketones, are normally characterised by a low chemoselectivity. This derives from the numerous possibilities for initiation and termination reactions which lead to different catalytic cycles and from facile multiple alternating insertion reactions of olefins and carbon monoxide. Based on experiments carried out under conditions of low selectivity and on previously published data, the factors involved in the control of the regio-, chemo- and stereoselectivity for those reactions are discussed, taking current ideas and model studies involving the above palladium complexes into consideration.
    Additional Material: 3 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19971301103
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  • 194
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    Cobalt Phthalocyanine Derivatives Supported on TiO2 by Sol-Gel Processing. Part 1: Preparation and Microstructure (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1585-1589 
    Details
    ISSN: 0009-2940
    Keywords: Phthalocyanines ; Sol-gel processes ; Titanium alkoxides ; Supported catalysts ; Heterogenous catalysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cobalt(II) 2,9,16,23-tetrasulphophthalocyanine and cobalt(II) 2,9,16,23-tetra(chlorosulphonyl)phthalocyanine were supported on TiO2 by reaction of the phthalocyanines with Ti(OR)4 followed by sol-gel synthesis. The thus obtained solid materials are stable in sulfide-containing media and are therefore suitable as catalysts for HS oxidation. The structure of the samples was characterized by electron microscopy diffraction. The morphology of the matrix strongly depends on the cobalt phthalocyanine derivative. The pathalocyanines in the titania matrices are monomeric or dimeric depending both on the type of substituents of the CoPc derivative and on the titanium alkoxide used as precursors.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971301106
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  • 195
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    Dichlorogermylene-Alkyldichlorophosphane Reactions Revisited: Characterisation of Bis(trichlorogermyl)phosphanes, Trichlorogermyldiphosphanes, and Ge-P Heterocycles (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1611-1618 
    Details
    ISSN: 0009-2940
    Keywords: Alkyldichlorophosphanes ; Insertions ; Carbene homologues ; Germanium ; Phosphonium germanate(II) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions of alkyldichlorophosphanes 1 (RPCl2; R = tert-butyl: 1a, R = isopropyl; 1b, R = 1-adamantyl: 1c) with the germanium dichloride dioxane complex were followed by 31P NMR. Depending on the organic substituents and the reaction conditions, mixtures of trichlorogermylphosphanes RP(GeCl3)2 4a-c, RPHGeCl3 5a-c, diphosphanes R(H)PP(H)GeCl3 6a-c, R(Cl)PP(H)GeCl3 7a, b cyclophosphanes, and Ge-P heterocycles such as triphosphadigermolanes (RP)3(GeCl2)2 8a, b and tetraphosphagermolane (RP)4)GeCl2 10b are formed. As a further unexpected byproduct of the reaction of 1a with GeCl2-dioxane, a small amount of tri-tert-butyl(trichlorogermyl)cyclotetraphosphane 9a was isolated. From the reaction of 1c with two equivalents of GeCl2-dioxane, separation from byproducts 5c and 6c by crystallisation furnished colourless crystals of 4c (R = 1-adamantyl) as the first pure organylbis(trichlorogermyl)phosphane. Surprisingly, the reaction of isoprophylphosphane with germanium tetrachloride, intended to prepare 5a, led to crystalline isopropylphosphonium trichlorogermanate(II) 11. The structures of molecular 4c and 9a and ionic 11 were determined by X-ray crystallography.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301109
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  • 196
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    Investigation of Host-Guest Interactions between Rubidium Salts and N-(Arylazoalkenoyl)azacoronands by Solid-State NMR SpectroscopyDedicated to Professor Dr. Reiner Radeglia on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1625-1627 
    Details
    ISSN: 0009-2940
    Keywords: N-(Arylazoalkenoyl)azacoronands ; Rubidium Salts ; Host-guest interaction ; 87Rb MAS NMR spectroscopy ; 13C CPMAS NMR spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Rubidium salts with N-(Arylazoalkenoyl)azacoronands (2a-c), were investigated using 87Rb and 13C solid-state NMR spectroscopy. From the NMR results it is concluded that there is a host-gust interaction. This suggests that the rubidium and ammonium ions, respectively, are incorporated into the cavity between the coronand and the chromophore.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301111
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    Synthesis and Structure of Trimethyllead Niobocene DihydrideDedicated to Professor Jörg Lorberth on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1629-1631 
    Details
    ISSN: 0009-2940
    Keywords: Lead ; Niobium ; Hydrides ; Group 5 ; Group 14 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of niobocene trihydride [Cp2NbH3] with ClPbMe3 in the presence of amine affords the plumbido dihydride complex [Cp2NbH2(PbMe3)] (1). Compound 1 represents the first example of a stable complex with neighbouring hydride and terminal plumbyl substituents. The structure of this compound has been established by NMR and IR spectroscopy and confirmed by an X-ray structure analysis.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301112
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  • 198
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    Steric Effects on Base Adduct Formation and Crystal Structures of Diastereomers of a Nickel(II) Schiff Base Complex (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1643-1646 
    Details
    ISSN: 0009-2940
    Keywords: Nickel Schiff base complexes ; Base adducts ; Chirality ; Steric hindrance ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of the ligand meso-H2L, derived from cis-diaminocyclohexane and ethyl cyano(ethoxymethylene)acetate, with nickel(II) acetate gives meso-NiL. Spectrophotometric titration of RR-NiL and meso-NiL with various nitrogen bases reveals a strong influence of the steric hindrance of the diaminocyclohexanediyl bridge in meso-NiL on the base adduct stability. The structures of RR-NiL and meso-NIL have been established by X-ray diffraction.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301114
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  • 199
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    Chlorides and Acetylacetonates of Transition Metals as Catalysts for the Oxidation of 1-Indanol by Sodium Percarbonate (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1655-1658 
    Details
    ISSN: 0009-2940
    Keywords: Catalysis ; Oxidations ; Transition metals ; Sodium percarbonate ; 1, 2-Dichloroethane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The screening of metal chlorides and metal acetylacetonates as catalysts for the oxidation of 1-indanol by sodium percarbonate (at reflux in 1,2-dichloroethane in the presence of small amounts of Adogen 464) has been carried out. The efficiency of the process depended on the nature of the transition metal and its oxidation state but, except for iron, was not greatly influenced by the nature of the ligands. Good conversions and yields have been obtained using PdCl2, RhCl3, RuCl3 and, particularly, MoO2(acac)2 as catalysts.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301116
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    Metal Complexes of Biologically Important Ligands, XCIV. Hexanuclear Isocyanide and Carbene Metal Complexes from Neomycin BDedicated to Professor Armin Weiß on the occasion of his 70th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1659-1662 
    Details
    ISSN: 0009-2940
    Keywords: Hexadeamino-hexaisocyano-neomycin B ; Organometallic complexes ; Gold ; Chromium ; Rhodium ; Iridium ; Ruthenium ; Palladium ; Platinum ; Hexanuclear carbene gold(I) complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: From the amino glycoside neomycin B, the acetate-protected hexaisocyanide 4 has been prepared. 4 forms the hexanuclear complexes [(4)(AuCl)6] (5), {(4)[Cr(CO)5]6}, {(4)[MCl2(η5-C5Me5)]6} (M = Rh, Ir), {(4)[RuCl2(p-cymene)]6}, {(4)-[MCl2(PR3)]6} (M=Pd, Pt), and 4{(4)[PdCl(C6H4CH2NMe2)]6). The hexaisocyanohexagold(I) complex 5 reacts with H2NtBu and PhNH2 to give the corresponding carbene complexes. The compounds have been characterized by IR, 13C- and 31P-NMR spectroscopy, and (partially) by FAB-MS data.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301117
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