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  • 1990-1994  (10)
  • 1970-1974  (2)
  • Inorganic Chemistry  (11)
  • Aurate(I), bis[2,4,6-tri(isopropyl)thiophenolato] ammonium  (1)
  • Organic Chemistry  (1)
  • 1
    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Crystal Structure of the First Quinoid Dihydropterinmolybdenum (IV) ComplexThe first molybdenum(IV) complex with a quinoid dihydropterin, i.e. 2, was isolated and characterized by IR, UV and NMR data and single-crystal X-ray diffraction. The reaction of MoVIO2Cl2 with the biologically important 6β-5,6,7,8-tetrahydro-L-biopterin(2) (7) in MeOH gave almost quantitatively trichloro(1,5-quinoid-7,8-dihydro-6H-L-biopterin)oxomolybdenLim(IV) (2). The complex crystallizes with one molecule of MeOH in the noncentrosymmetric orthorhombic space group P212121 (No. 19) with unit cell dimensions a = 1009.3(3), b = 1104.7(3), and c = 1484.5(4) pm and Z = 4. The Mo-atom has a distorted octahedral geometry (Fig.1). It is coordinated by N(5) and O(4) of the pterin ligand. The distance of the Mo-N(5) bond (202 pm) is unusually short compared to similar complexes. O(4) is located trans to a terminal oxo ligand. The octahedral coordination is completed by three Cl-atoms in a meridional arrangement. Complex 2, with the Mo-atom in the enzyme-relevant oxidation state +IV and the pterin in the intermediate quinoid dihydro form, should lead to an extension of the proposed ‘common molybdenum cofactor’ model.
    Additional Material: 3 Ill.
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  • 2
    ISSN: 0009-2940
    Keywords: Lithium dicyanomethanide ; Sodium dicyanomethanide ; Dicyanomethanides, lithium, sodium, tetrabutylammonium salts ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Crystal Structures of {Li3(12-crown-4)2[HC(CN)2]3}, {Na(15-crown-5)[HC(CN)2]}, and {NaN(nBu)4[HC(CN)2]2 · THF}The preparation and the crystal structures of the title compounds 1 - 3 are described. 1 forms a polymeric chain structure, in which one of the lithium ions is linked by Li…NCC(H)CN… bridges. The remaining lithium ions form (12-crown-4)Li[NCC(H)CN] units, which are coordinated by one of the nitrogen atoms of the dicyanomethanide ions with the lithium ions of the chain. 2 forms an ion pair, in which the sodium ion is coordinated by the five oxygen atoms of the crown ether molecule and by one nitrogen atom of the dicyanomethanide ion. 3 has a threedimensional network, in which the sodium ions are coordinated in a distorted tetrahedral manner by the nitrogen atoms of the dicyanomethanide ions. In the cavities of the network the tetrabutylammonium ions and the THF molecules are found.
    Additional Material: 3 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 2161-2164 
    ISSN: 0009-2940
    Keywords: Gold(I) 2,4,6-tri(isopropyl)thiophenolate, hexamer ; Aurate(I), bis[2,4,6-tri(isopropyl)thiophenolato] ammonium ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thiolato Complexes of Monovalent Gold. Synthesis and Structure of [(2,4,6-iPr3C6H2S)Au]6 and (NH4)[(2,4,6-iPr3C6H2S)2Au]Reaction of Au(CO)Cl with 2,4,6-tri(isopropyl)thiophenol affords hexameric gold(I) thiolate [(2,4,6-iPr3C6H2S)Au]6 (1). According to an X-ray analysis 1 forms a centrosymmetrical twelve-membered Au - S ring in the chair conformation with the linearly coordinated Au atoms at the mid-edges and the S atoms at the corners of the heterocycle. When the reaction of 2,4,6-tri(isopropyl)thiophenol is carried out with AuI in liquid ammonia the thiolato complex [(2,4,6-iPr3C6H2S)2Au]- -NH+4 (2) is obtained. It crystallizes as NH4 · 2 · 3 NH3. The gold atom in 2 is linearly coordinated by two thiolato S atoms. The ammonium cation forms hydrogen bonds with three NH3 solvate molecules.
    Additional Material: 2 Ill.
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  • 4
    ISSN: 0009-2940
    Keywords: Bis-arene complexes ; Niobium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bis(mesitylen)niobium(0), Nbmes2, prepared via the NbCl5/Al/AlCl3/mes system by exaustive reduction in the presence of 1,2-dimethoxyethane or tetrahydrofuran as previously reported, has been studied by X-ray diffraction methods. The sandwich molecule has parallel, substantially planar, aromatic rings, in an eclipsed conformation. Nbmes2 is oxidized to Nbmes2X by reaction with 1,1-dimethyl-4,4′-bipyridinium halides [methylviologen halides, mvX2 (X = Cl, I)]. The reaction of both halo compounds with CO yielded the niobium(I) derivatives [Nbmes2(CO)] [Nb2(μ-X)3(CO)8]. In the case of X = I an IR study at low temperature has shown the presence of intermediate carbonyl compounds, presumably Nbmes2I(CO) and [Nbmes2(CO)]+. The ionic iodide derivative was shown by X-ray diffraction methods to consist of discrete [Nbmes2(CO)]+ cations and [Nb2(μ-I)3(CO)8]- anions. The two mesitylene groups in the cation are bent and in an eclipsed conformation.
    Additional Material: 6 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1597-1605 
    ISSN: 0009-2940
    Keywords: Polymers, low-gap ; Polyarenemethines ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of suitable precursors of polyarenemethines (PAM) 1, which are predicted to be potential low gap polymers, is described. The Knoevenagel condensation of heteroaromatic aldehydes with 2,5-dihydrothiophene 1,1-dioxide (5), 2,5-dihydrothiophene 1-oxide (9), and its benzo-annulated analogs [6 and [10] yields the methine-bridged compounds 7, [8], 11, and [12], respectively. Reduction of the methine-bridged sulfoxides 11 and [12] leads to the corresponding sulfides 13 and [14]. For compound 18 with a high sterical demand another route has been developed. Thus, the reaction of the dicarbinol 17 with HI yields directly the heteroaromatic quinodimethane 18. The molecular structures of 7a and 18 are determined by X-ray analysis.
    Additional Material: 3 Ill.
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  • 6
    ISSN: 0044-2313
    Keywords: Phosphaneiminato complexes of Nb, Mo, W ; reactions with NaF ; triphenylaminophosphonium chloride ; triphenyl-difluorophosphorane ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reactions of Phosphaneiminato Complexes of Niobium, Molybdenum, and Tungsten with Sodium Fluoride. The Crystal Structures of [PPh3NH2]Cl and PPh3F2[NbCl4(NPPh3)]2 reacts with excess sodium fluoride and 15-crown-5 in acetonitrile, forming the fluoro complex [Na-15-crown-5][NbF5(NPPh3)] at room temperature. In boiling acetonitrile the solvent takes part in the cleavage of the Nb—N bond of the phosphaneiminato complex, yielding [PPh3NH2]Cl. In corresponding reactions the phosphaneiminato complexes [MoCl4(NPPh3)]2 and [WCl5(NPPh3)] undergo a cleavage of the P—N bond giving PPh3F2 in a good yield. [PPh3NH2]Cl and PPh3F2 are characterized by crystal structure analyses:[PPh3NH2]Cl: Space group Pna21, Z = 4,1796 observed independent reflexions, R = 0.030. Lattice constants at -60°C: a = 1084.7, b = 961.7, c = 1536.5. The compound consists of PPh3NH2+ ions and chloride ions, which link the cations to … HNH … Cl … HNH … Cl chains.PPh3F2: Space group Pbcn, Z = 4,987 observed independent reflexions, R = 0.044. Lattice constants at 20°C: a = 611.41, b = 1664.2, c = 1436.9. This compound has a trigonal bipyramidal structure with the fluorine atoms in the axial positions.
    Notes: Die Reaktion von [NbCl4(NPPh3)]2 mit überschüssigem Natriumfluorid in Acetonitril führt in Gegenwart von 15-Krone-5 in der Kälte zu dem Fluorokomplex [Na-15-Krone-5][NbF5(NPPh3)]. In der Siedehitze findet unter Mitwirkung des Lösungsmittels Spaltung der Nb—N-Bindung des Phosphaniminatokonplexes statt, wobei [PPh3NH2]Cl gebildet wird. Entsprechende Untersuchungen mit den Phosphaniminatokomplexen [MoCl4(NPPh3)]2 und [WCl5(NPPh3)] führen unter Spaltung der P—N-Bindung zu PPh3F2, das in guter Ausbeute erhalten wird. [PPh3NH2]Cl und PPh3F2 haben wir durch Kristallstrukturanalysen charakterisiert.[PPh3NH2]Cl: Raumgruppe Pna21, Z = 4,1796 unabhängige, beobachtete Reflexe, R = 3,0%. Gitterkonstanten bei -60°C: a = 1084,7; b = 961,7; c = 1536,5 pm. Die Verbindung besteht aus PPh3NH2+-Ionen und Chloridionen, die über Wasserstoffbrückenbindungen … HNH … Cl … HNH … Cl die Kationen zu Ketten verknüpfen.PPh3F2: Raumgruppe Pbcn, Z = 4,987 unabhängige, beobachtete Reflexe, R = 4,4%. Gitterkonstanten bei 20°C: a = 611,41; b = 1664,2; c = 1436,9 pm. Die Verbindung hat eine trigonal-bipyramidale Molekülstruktur mit den Fluoratomen in den Axialpositionen.
    Additional Material: 2 Ill.
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  • 7
    ISSN: 0044-2313
    Keywords: Triphenylarsin-p-toluene sulfonylimine ; Zirconium tetrachloride complex ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structures of Triphenylarsin-p-toluene Sulfonylimine and of its Donor-Acceptor Complex [ZrCl4(Ph3AsNSO2Tol)]2The molecular structures of the title compounds are reported. In the donor-acceptor complex [ZrCl4(Ph3AsNSO2Tol)]2 the zirconium atoms are bridged by the oxygen atoms of the triphenylarsin-p-toluene sulfonylimine molecules, forming a centrosymmetric dimer with a puckered Zr2O4S2 eight-membered ring in the chair conformation.Ph3AsNSO2Tol: Space group P1, Z = 2, structure determination with 4 010 observed unique reflections, R = 0.036. Lattice dimensions at 19°C: a = 897.52(4), b = 1 071.82(6), c = 1 337,49(5) pm, α = 110.280(4)°, β = 98.814(4)°, γ = 109.872(4)°.[ZrCl4(Ph3AsNSO2Tol)]2: Space group P21/n, Z = 4, structure determination with 3 762 observed unique reflections, R = 0.078. Lattice dimensions at -60°C: a = 1 387.3(4), b = 1 434.9(2), c = 1 404.7(4) pm, β = 92.71(1)°.
    Notes: Es wird über die Molekülstrukturen der beiden Titelverbindungen berichtet. In dem Donor-Akzeptorkomplex [ZrCl4(Ph3AsNSO2Tol)]2 sind die Zirkoniumatome über die O-Atome der Triphenylarsin-p-toluolsulfonylimin-Moleküle zu einem zentrosymmetrischen Dimer mit einem Zr2O4S2-Achtring in der Sesselkonformation verknüpft.Ph3AsNSO2Tol: Raumgruppe P1, Z = 2, Strukturlösung mit 4 010 unabhängigen beobachteten Reflexen, R = 0,036. Gitterkonstanten bei 19°C: a = 897,52(4), b = 1 071,82(6), c = 1 337,49(5) pm, α = 110,280(4)°, β = 98,814(4)°, γ = 109,872(4)°.[ZrCl4(Ph3AsNSO2Tol)]2: Raumgruppe P21/n, Z = 4, Strukturlösung mit 3 762 unabhängigen beobachteten Reflexen, R = 0,078. Gitterkonstanten bei -60°C: a = 1 387,3(4), b = 1 434,9(2), c = 1 404,7(4) pm, β = 92,71(1)°.
    Additional Material: 2 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 91-96 
    ISSN: 0044-2313
    Keywords: Lithium chloride crown ether complex ; I.R. spectrum ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Li(12-Crown-4)]Cl: Crystal Structure and I.R. SpectrumColourless single crystals of [Li(12-crown-4)]Cl were obtained from acetonitrile solutions of LiCl in the presence of 12-crown-4. They were characterized by i. r. spectroscopy as well as by an X-ray structure determination. Space group P4/n, Z = 2, 1 080 observed unique reflections, R = 0.034. Lattice dimensions at -50°C; a = 837.8(5), c = 752.0(2) pm. [Li(12-crown-4)]Cl forms ion pairs with tetragonal symmetry and bond lengths Li—O of 212.8 pm and Li—Cl of 229.0 pm.
    Notes: [Li(12-Krone-4)]Cl wurde aus LiCl-Lösungen in Acetonitril in Gegenwart von 12-Krone-4 in farblosen Einkristallen erhalten, die durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert werden. Raumgruppe P4/n, Z = 2, 1080 beobachtete unabhängige Reflexe, R = 3,4%. Gitterabmessungen bei -50°C: a = 837,8(5), c = 752,0(2) pm. [Li(12-Krone-4)]Cl bildet Ionenpaare mit tetragonaler Symmetrie und Abständen Li—O von 212,8 pm und Li—Cl von 229,0 pm.
    Additional Material: 2 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 375 (1970), S. 238-254 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: MoNCl3 crystallises in the triclinic space group PI with 4 formula units per unit cell, the lattice constants being a = 9.14, b = 7.67, c = 8.15 Å; α = 108.8°, β = 99.3° and γ = 108.6°. The crystal structure was solved by means of three-dimensional PATTERSON and FOURIER syntheses and refined by the method of least squares to a reliability index of 5.8%. The structure is built up from two slightly different kinds of MoNCl3 molecules having Mo—N triple bonds (Mo—N distances 1.64 and 1.67 Å). Each N atom is coordinated to the Mo atom of a neighbouring molecule in such a way that tetramers with the pseudosymmetry 4/m are formed. The tetramers are linked together by bridging Cl atoms so that puckered layers parallel to (010) result.
    Notes: MoNCl3 kristallisiert triklin (Raumgruppe PI) mit 4 Formeleinheiten pro Elementarzelle und den Gitterkonstanten a = 9,14, b = 7,67, c = 8,15 Å; α = 108,8°, β = 99,3° und γ = 108.6°. Die Kristallstruktur wurde aus dreidimensionalen PATTERSON und FOURIER-Synthesen abgeleitet und nach der Methode der kleinsten Quadrate bis zu einem Zuverlässigkeitsindex von 5,8% verfeinert. Die Struktur baut sich aus zwei wenig verschiedenen Arten von MoNCl3-Molekeln auf, die Mo—N-Dreifachbindungen enthalten (Mo—N-Abstände 1,64 und 1,67 Å). Jedes N-Atom ist in der Weise zum Mo-Atom einer Nachbarmolekel koordiniert, daß Tetramere mit der Pseudosymmetrie 4/m entstehen. Die Tetrameren sind durch Cl-Brücken lose verknüpft und bilden gewellte Schichten parallel zu (010).
    Additional Material: 2 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 380 (1971), S. 96-96 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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