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  • 1
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Silicon-Sulfur Compounds. XXXVI. Mercury(II)-bis-tri-tert-butoxysilanethiolateMercury(II)bis-tri-tert-butoxysilanethiolate was obtained in reaction of HgO with (t-C4H9O)3SiSH. This compound forms colourless triclinic plates. The central S—Hg—S bond element is linear, with Hg—S bond distance of 231.6 pm. The Hg atom is coordinated by two oxygens of the two butoxy groups, with Hg—O distance of 287.8 pm. The mean bond angle at the two-bonded sulfur is 95.6°. (Space group P1; a = 930.8, b = 944.0, c = 1204.8 pm, α = 100.34, β = 97,64, γ = 116.50°; Z = 1; R = 0.035; 3390 reflections hkl).
    Notes: Quecksilber(II)-bis-tri-t-butoxysilanthiolat wurde in einer Umsetzung von HgO mit (t-C4H9O)3SiSH erhalten. Die Verbindung kristallisiert in farblosen, triklinen Plättchen. Die zentrale S—Hg—S Bindungseinheit ist linear mit d(Hg—S) = 231,6 pm. Das Hg-Atom ist von O-Atomen der tert-Butoxygruppen koordiniert, d(Hg—O) = 287,8 pm. Der Bindungswinkel am zweibindigen Schwefel beträgt 95,6°. (Raumgruppe P1; a = 930,8, b = 944,0, c = 1204,8 pm, α = 100,34, β = 97,64, γ = 116,50°; Z = 1, R = 0,035; 3390 Reflexe hkl).
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  • 2
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of Tetrafluoro(η5-pentamethylcyclopentadienyl) Niobium and Tetrafluoro(η5-cyclopentadienyl) NiobiumA facile preparation method for (η5-C5Me5)NbF4 3 and (η5-C5H5)NbF4 4 is reported by using AsF3 as a fluorinating agent. Single crystals obtained from AsF3 contain the solvent molecule as well as HF. The composition of the crystal is [(η5-C5Me5)NbF4(AsF3)2]2 · [(η5-C5Me5)NbF4(HF)AsF3]2 5. The X-ray crystal structure of 5 will be reported. 5 crystallizes triclinic with one furmula in the space group P1 and lattice constants a = 843.1(4), b = 1154.9(6), c = 1910.2(10) pm, α = 91.68(3)°, β = 99.30(3)°, γ = 104.44(2)°.
    Notes: Es wird über eine einfache Darstellung von (η5-C5Me5)NbF4 3 und (η5-C5H5)NbF4 4 durch Chlor-Fluor Austausch mittels AsF3 berichtet. 3 kristallisiert mit AsF3 und HF als [(η5-C5Me5)NbF4(AsF3)2]2 · [(η5-C5Me5)NbF4(HF)AsF3]2 5 aus. Die Einkristall Röntgenstrukturanalyse von 5 wird mitgeteilt. 5 kristallisiert triklin in der Raumgruppe P1 mit den Gitterkonstanten a = 843,1(4), b = 1154,9(6), c = 1910,2(10) pm und α = 91,68(3)°, β = 99,30(3)°, γ = 104,44(2)° mit einer Formeleinheit in der Elementarzelle.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 118 (1985), S. 2659-2670 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Hexafluoroacetone with Alkali CyanatesNaSCN and KOCN react with hexafluoroacetone (HFA) in a molar ratio of 1:2 in a one-step reaction to yield the hexafluoropropanimine derivatives (CF3)2C=NC(CF3)2OM (2a, b) (M=Na, K). (CF3)2C=N- is a possible intermediate. Hydrolysis of 2a in aqueous tetraphenylphosphonium chloride solution yields a crystalline hydrate of composition [(CF3)2C(OH)2·(CF3)2C(O)OH]- Ph4P+ (3). In the solid state dimeric dianions are observed, which are connected via four asymmetrical and two symmetrical O⃛H⃛O bonds. Starting with a 1:1 KSCN/HFA stoichiometry the polycyclic bisspiro compound 5 is formed in a complex reaction. In the reaction of potassium selenocyanate with HFA the C-Se bond is cleaved and the CF3-substituted oxazolidine 6 is formed. The X-ray structure analyses of 2a, 3, 5 and 6 are reported.
    Notes: NaSCN und KOCN reagieren mit Hexafluoraceton (HFA) im Molverhältnis 1:2 unter Abbau des Anions in einem Schritt zu den Hexafluorpropanimin-Derivaten (CF3)2C=NC(CF3)2OM (2a, b) (M=Na, K), wahrscheinlich über (CF3)2C=N- als Zwischenstufe. Die Hydrolyse von 2a in Gegenwart wäßriger Tetraphenylphosphoniumchlorid-Lösung ergibt ein kristallines Hydrat der Zusammensetzung[(CF3)2C(OH)2·(CF3)2C(O)OH]- Ph4P+ (3). Im Kristall liegen dimere Dianionen vor, die über vier asymmetrische und zwei symmetrische Wasserstoff-Brückenbindungen verknüpft sind. In einer unübersichtlichen Reaktion entsteht bei einem Reaktandenverhältnis KSCN/HFA von 1:1 die polycylische Bisspiroverbindung 5. Kaliumselenocyanat reagiert mit HFA unter C - Se-Bindungsspaltung und nachfolgender Bildung des CF3-substituierten Oxazolidins 6. Die Röntgenstrukturanalysen von 2a, 3, 5 und 6 werden mitgeteilt.
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  • 4
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of S, S-Diphenyl-N-(trimethylsilyl)sulfimine and Reactions with Tungsten Hexafluoride - X-Ray Structure Analysis of F4W(N=SPh2)Ph2S=NH reacts with Me3SiNMe2 to give S,S-diphenyl-N-(trimethylsilyl)sulfimine (1) in a metathesis. Reaction of WF6 with 1 in a 1:1 molar ratio leads to F5WN=SPh2 (2); a 1:2 molar ratio results in the formation of F4W(N=SPh2)2 (3). The structure of 3 is confirmed by an X-ray analysis.
    Notes: Aus Ph2S=NH wird mit Me3SiNMe2 durch Metathese S,S-Diphenyl-N-(trimethylsilyl)sulfimin (1) erhalten. WF6 reagiert mit 1 im Molverhältnis 1:1 zu F5WN=SPh2 (2) und im Molverhältnis 1:2 zu F4W(N=SPh2)2 (3). Von 3 wird eine Röntgenstrukturanalyse vorgelegt.
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  • 5
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Benzamidinato Complexes of Main Group and Transition Metals - Crystal Structures of PhC(NSiMe3)2TiCl2 and PhC3)2MoO2PhC(NSiMe3)2Li (3b) reacts with SiCl4, SnCl4, Me2SnCl2, Ph2SnCl2, TiCl4, ZrCl4, MoO2Cl2, and WO2Cl2 with formation of LiCl to yield the new amidinato complexes 4a-f, 5a and 5b. The X-ray structure analyses of 4e and 5a are reported.
    Notes: PhC(NSiMe3)2Li (3b) reagiert mit SiCl4, SnCl4, Me2SnCl2, Ph2SnCl2, TiCl4, ZrCl4, MoO2Cl2 und WO2Cl2 unter Bildung von LiCl zu den Amidinatokomplexen 4a-f, 5a und 5b. Von 4e und 5a wird die Röntgenstrukturanalyse mitgeteilt.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 63-65 
    ISSN: 0009-2940
    Keywords: Silicon - nitrogen cleavage ; Tungsten heterocycles containing N, P, and S ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Heterocycles Containing Tungsten, Phosphorus, Sulphur, and Nitrogen in the Ring SkeletonThe new ligand Me2S(NPPh2NSiMe3)2 (2), prepared from Me2S-(NPPh2)2 (1) and Me3SiN3, reacts with WF6 and WCl6 to form the heterocycles Me2S(NPPh2N)2WF4 (3a) and Me2S(NPPh2N)2WCl4 (3b). The X-ray single-crystal structure analysis exhibits a puckered eight-membered ring with alternating short and long bond lengths. 3a crystallizes with one molecule of dimethylformamide in the space group Cc with a = 1247.3(6), b = 1728.5(9), c = 1543.1(8) pm and β = 102.41(3)°.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 123 (1990), S. 691-696 
    ISSN: 0009-2940
    Keywords: Thioacetone, hexafluoro-/1,2,4-Dithiazolines/1,2,4-Thiaselenazolines ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New Syntheses of Trifluoromethyl-Substituted HeterocyclesDimeric hexafluorothioacetone (HFTA) (1) reacts with thiourea or phenylthiourea to give 1,2,4-dithiazolines 2a and 2b. Similarly, 1,2,4-thiaselenazoline 3 is obtained from the reaction of 1 with selenourea. Reaction of 1 with oxamic hydrazide or thiosemicarbazide leads to acyclic molecules 4 and 5. Besides 5, the cyclic isomer 6 is also observed in solution. The N-trifluoroacetyl derivative 6a is obtained from the reaction of 5 with trifluoracetic anhydride. The structures of 2b, 3, 5, and 6a have been determined by single-crystal X-ray crystallography.
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  • 8
    ISSN: 0009-2940
    Keywords: Bulky substituents ; Aluminum compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Structure of CpAlCl2 Compounds with Sterically Demanding Substituents (Cp = Me5C5, EtMe4C5)[1]The compounds Cp*AlCl2 (3) (Cp* = Me5C5) and Cp′AlCl2 (4) (Cp′ = EtMe4C5) have been prepared by the reaction of Cp*SiMe3 (1) and Cp′SiMe3 (2) with AlCl3. The single-crystal X-ray structures of 3 and 4 are reported.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 2359-2361 
    ISSN: 0009-2940
    Keywords: Rhenium(VII) compounds ; Organooxides of elements of group 14 and 15 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New Perrhenates and Aminorhenium Trioxides with Elements of Group 14. and 15. of the Periodic SystemNew perrhenates have been prepared by reaction of Re2O7 with triphenylstibin oxide and di-n-butyltin oxide, respectively. The single-crystal X-ray structure of Ph3Sb(OReO3)2 (1) is reported. The reaction of Ph3SbO and nBu2SnO with Re2O7 in 1:2 molar ratio gives (O3ReOSbPh3)2O (2) and [O3ReOSn-(nBu)2]2O (3), respectively. A trimethylstannyl-substituted aminorhenium trioxide (Me3Sn)2NReO3 (4) has been prepared by reaction of Me3SiOReO3 and N(SnMe3)3.
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  • 10
    ISSN: 0009-2940
    Keywords: Molybdenum(VI) compound ; Siloxanes ; Vanadium(V) compound ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Model Reactions to Anchor Molybdenum and Vanadium Oxides on Silica-Oxygen SurfacesThe eight-and twelve-membered ring compounds [(tBu)21-Si(O)2MoO2]2 (1) and [(tBu)2Si(O)2V(O)Cl]3 (2) have been prepared by the reaction of di-tert1-butylsilanediol or its dilithium salt with MoO2Br2 or VOCl3, respectively. Single crystal X-ray structure analyses of 1 · 2 py and 2 have been performed. Crystals of 1 · 2 py contain two molecules of 1 · 2 py and four additional molecules of pyridine in the unit cell.
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