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  • Articles  (92)
  • Inorganic Chemistry  (92)
  • Wiley-Blackwell  (92)
  • American Meteorological Society
  • 1995-1999  (92)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1385-1394 
    ISSN: 0044-2313
    Keywords: Palladium ; quaternary fluorides ; LiPdGaF6 ; RbPdAlF6 ; K1.06Pd0.95Fe1.05F6 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of LiPdGaF6, RbPdAlF6 and K1.06Pd0.95Fe1.05F6Single crystals of LiPdGaF6 (blue; trigonal, P31c-D3d2 (No. 163), a = 505.72(2), c = 923.7(2) pm; LiCaAlF6-Type [1]), RbPdAlF6 (violet; orthorhombic, Pnma-D2h16 (No. 62), a = 729.0(1), b = 711.1(1), c = 1006.5(2) pm; CsAgFeF6-Type [2]) and K1.06Pd0.95Fe1.05F6 (greenish-blue; tetragonal, P42/mbc-D4h13 (No. 135), a = 1 279.07(7), c = 800.2(1) pm; K1,08MnFeF6-Type [3]; four cycle diffractometer data, Siemens AED2) are obtained by heating the binary fluorides in sealed Pd-tubes under dry argon [solid state reaction, T ≈ 650, t ≈ 19 d (39 d, 24 d)].
    Notes: Durch Umsetzung von äquimolaren Gemengen der binären Fluoride im verschweißten Pd-Rohr unter Schutzgas [Ar, Festkörperreaktion, T = 650°C, t = 19 d (39 d, 24 d)] erhält man Einkristalle von LiPdGaF6 (blau, trigonal, P31c-D3d2 (No. 163), a = 505,72(2), c = 923,7(2) pm, LiCaAlF6-Typ [1]), RbPdAlF6 (violett, orthorhombisch, Pnma-D2h16 (No. 62), a = 729,0(1), b = 711,1(1), c = 1006,5(2) pm, CsAgFeF6-Typ [2]) sowie K1,06Pd0,95Fe1,05F6 (blau-grün, tetragonal, P42/mbc-D4h13 (No. 135), a = 1279,07(7), c = 800,2(1) pm; K1,08MnFeF6-Typ [3]; jeweils Vierkreisdiffraktometerdaten).
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1047-1052 
    ISSN: 0044-2313
    Keywords: Zirconium fluoride ; hafnium fluoride ; ternary fluorides ; KPdMIVF7 (MIV = Zr, Hf) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of KPdMIVF7 (MIV = Zr, Hf)Blue single crystals of KPdZrF7 are obtained by heating the binary fluorides in sealed Pt-tubes under dry argon (solid state reaction, T ≍ 720°C, t ≍ 14 d). The compound crystallizes orthorhombically in the space group Pnna-D2h6 (Nr. 52); lattice parameters are a = 1 132.3(5) pm, b = 797.5(2) pm, c = 639.8(1) pm; Z = 4 (Four cycle diffractometer data, AED2). According to [F4PdF2/1ZrF5] distortet [PdF6]-octaedra are connected with pentagonal-bipyramidal [ZrF7]-polyhedra via two bridging F-, resulting in [PdZrF11]-groups. These [PdZrF11]-groups built up a threedimensional-network with K+ in its spacings. KPdHfF7 crystallizes isotypically (a = 1 136.1(3) pm, b = 796.4(2) pm und c = 638.8(1) pm; four cycle diffractometer data, AED2).
    Notes: Durch Tempern der binären Fluoride im verschweißten Pt-Rohr unter Schutzgas (Ar, Festkörperreaktion, T ≍ 720°C, t ≍ 14d) erhält man blaue Einkristalle von KPdZrF7 [eigener Strukturtyp, orthorhombisch, Pnna-D2h6 (Nr. 52); a = 1 132,3(5) pm, b = 797,5(2) pm, c = 639,8(1) pm; Z = 4; Vierkreisdiffraktometerdaten AED2]. Pd2+ ist verzerrt oktaedrisch von 6 F- umgeben, wohingegen Zr4+ pentagonalbipyramidal von 7 F- koordiniert wird. Beide Koordinationspolyeder sind gemäß [F4PdF2/1ZrF5] kantenverknüpft und bilden mit weiteren solcher [PdZrF11]-Einheiten durch Eckenverknüpfung ein dreidimensionales Raumnetz, in dessen Lücken K+ eingelagert ist. Nach Vierkreisdiffraktometerdaten (AED2) kristallisiert KPdHfF7 isotyp (a = 1 136,1(3) pm, b = 796,4(2) pm und c = 638,8(1) pm).
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 993-1000 
    ISSN: 0044-2313
    Keywords: Zirconium(IV) fluoride ; hafnium(IV) fluoride ; Cs2Cu3MIVF12 (MIV = Zr, Hf) ; crystal structure ; magnetic properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cs2Cu3MIVF12 (MIV = Zr, Hf) - Crystal Structure and Magnetic BehaviourColourless single crystals of Cs2Cu3ZrF12 are obtained by heating the binary fluorides in sealed Pt-tubes under dry argon (solid state reaction, T ≍ 700°C, t ≍ 7-10 d). The compound crystallizes trigonal-rhomboedrical in the space group R3m-D3d5 (Nr. 166); lattice parameters are a = 716.61(6) pm, c = 2 046.4(2) pm, Z = 3 (Four cycle diffractometer data, AED 2). The structure is dominated by layers of corner-sharing, Jahn-Teller-distorted [CuF6]-Octahedra, which are connected via regular [ZrF6]-Octahedra to stackings parallel [00.1]. Cs+-ions are located in the spacings of the octahedra-network. From powder data Cs2Cu3HfF12 with a = 716.32(4) pm, c = 2 048.6(2) pm is isotypic. Both compounds show antiferromagnetic behaviour already at temperatures about 200 K.
    Notes: Durch Umsetzung der binären Fluoride im verschweißten Pt-Rohr unter Schutzgas (Ar, Festkörperreaktion, T ≍ 700°C, t ≍ 20d) erhält man farblose Einkristalle von Cs2Cu3ZrF12. [Trigonal-rhomboedrisch, R3m-D3d5 (Nr. 166), a = 716,61(6) pm, c = 2 046,4(2) pm, Z = 3 (Vierkreisdiffraktometerdaten, AED 2)]. Strukturbestimmend sind Schichten eckenverknüpfter, Jahn-Teller-verzerrter [CuF6]-Oktaeder, welche - über reguläre [ZrF6]-Oktaeder verknüpft - Stapel entlang [00.1] bilden. In den Hohlräumen der Struktur sind Cs+-Ionen eingelagert. Nach Pulverdaten kristallisiert Cs2Cu3HfF12 mit a = 716,32(4) pm, c = 2 048,6(2) pm isotyp. Beide Stoffe zeigen bereits bei Temperaturen um 200 K antiferromagnetisches Verhalten.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1227-1231 
    ISSN: 0044-2313
    Keywords: TiF4 ; preparation, single crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Titanium Tetrafluoride - a Surprising Simple Column StructureFor the first time single crystals of TiF4 have been obtained by solvothermal decomposition of (O2)2Ti7F30 in anhydrous HF. The colourless, transparent needles crystallize orthorhombic in spacegroup Pnma-D2h16 (No. 62) with a = 2 281.1, b = 384.8, c = 956.8 pm, Z = 12. The new type of structure is dominated by isolated columns of corner-linked TiF6-octahedra.
    Notes: Durch Solvothermalsynthese in wasserfreier HF gelang es endlich erstmals, TiF4 aus (O2)2Ti7F30 in Form solcher Einkristalle darzustellen, die eine Strukturbestimmung ermöglichten. Die farblosen, transparenten Nadeln kristallisieren in der Raumgruppe Pnma-D2h16 (Nr. 62) mit a = 2 281,1, b = 384,8, c = 956,8 pm, Z = 12. TiF4 bildet einen eigenen Strukturtyp, dessen charakteristisches Merkmal von einander isolierte, aus TiF6-Oktaedern aufgebaute Säulen sind (Kolumnarstruktur).
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  • 5
    ISSN: 0009-2940
    Keywords: Reductive silylation ; Aminochlorophosphanes ; Silylphosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of alkyl(diorganylamino)chlorophosphanes R(R2′N)PCl 1 (1a: R = tBu, R′ = Et, 1b: R = iPr, R′ = iPr; 1c: R = iPr, R′ = Ph) with hexachlorodisilane, afforded alkyl(diorganylamino)trichlorosilylphosphanes R(R2′N)PSiCl3 2 (2a: R = tBu, R′ = Et; 2b: R = iPr, R′ = iPr; 2c: R = iPr, R′ = Ph) and silicon tetrachloride. An intermediate formed in the reaction of 1b with hexachlorodisilane, the adduct iPr(iPr2N)(Cl)P-Si(Cl)3-SiCl3 (3b = 1b · Si2Cl6), was detected by 31P- and 29Si-NMR spectra that indicate pentacoordinated silicon bound to tetracoordinated phosphorus and tetracoordinated silicon. Trichlorosilylphosphanes 2 are also available from 1 under very mild conditions by reductive trichlorosilylation with trichlorosilane in the presence of triethylamine. Compounds 2 were identified analytically, by mass spectroscopy, multinuclear NMR, and an X-ray structure determination of 2c.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 253-257 
    ISSN: 0009-2940
    Keywords: Lithiated phosphane imines ; Phosphane imines, lithiated ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Lithiated Phosphane Imines. Synthesis and Crystal Structures of [LiCH2PMe2NSiMe3]4 and [LiCMe2P(iPr)2NSiMe3]2The title compounds were prepared by the reaction of Me3-SiNPMe3 and Me3SiNP(iPr)3, respectively, with n-Butylli-thium at 20°C in n-hexane solution. They form white, moisture- and oxygen-sensitive crystals, which were characterized by IR spectroscopy and by crystal structure determinations. - [LiCH2PMe2NSiMe3]4 (1) forms a Li4 tetrahedron, the faces of which are capped with CH2 groups with average Li-C distances of 233 and 251 pm, while the nitrogen atoms occupy the corners of the Li4 tetrahedron. - [LiCMe2P(iPr)2N-SiMe3]2 (2) forms molecules of symmetry C2 in which the lithium atoms have coordination number three by two carbon atoms and one nitrogen atom with Li-C distances of 215.2 and 237.9 pm and Li-N of 192.8 pm.
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  • 7
    ISSN: 0009-2940
    Keywords: Phosphaalkenes ; Cycloadditions ; Insertion reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The dimethylamino-substituted phosphaalkene 1 reacts with hexafluoroacetone (HFA) with addition at the P=C bond to form the 1,5,2-dioxaphosphorinane 2. The structure of 2 was confirmed by an X-ray crystal structure analysis. The six-membered ring displays an envelope conformation with the phosphorus atom out of the plane, but the phosphorus is disordered over two sites. Reaction of P-trimethylsilyl-substituted phosphaalkenes with HFA proceeds with retention of the P=C double bond and insertion of HFA into the P—Si bond. Two isomeric products are obtained and are characterized by 1H-, 13C-, 19F-, and 31P-NMR spectroscopy, IR spectroscopy, mass spectrometry, and elemental analysis.
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  • 8
    ISSN: 0009-2940
    Keywords: Trichlorosilylation ; Dichlorophosphanes ; Silylphosphanes ; Amino(silyl)phosphanes ; Silicon /Reductions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of hexachlorodisilane and of trichlorosilane/triethylamine with alkyl-and dialkylaminodichlorophosphanes RPCl2 1a-i [R = iPr: a; (Me3Si)2CH: b; R=1-adamantly: c: R=tBu: d; R=Et2N: e; R=iPr2M: f] furnish bis(trichlorosilyl)-phosphanes RP(SiCl3)2 3a-f. However, when less bulky substituents are attached to the phosphorus atom, so that there is little steric crowding, the double reductive silylations leading from 1 to 3 are accompanied by side reactions and decomposition of 3. Therefore, only 3b, 3c, 3d, and 3f wre isolated in a pure state. These compounds are more readily prepared by the; trichlorosilane/triethylamine method. 1H-, 31P- and 29Si-Nmr spectra confirm their constitution. The structure of solid 3f, the first aminobis(trichlorosilyl)phosphane, was determined by X-ray crystallography. 3f contains a phosphorus atom in a pyramidal environment surrounded by two silicon atoms and a planar nitrogen atom of the diisopropylamino group.
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  • 9
    ISSN: 0009-2940
    Keywords: Porphyrinatomanganese(IV) ; Monooxygenase model ; Dichloro monoxide ; Catalytic alkene epoxidation ; Catalytic alkane oxygenation ; Catalytic alkane chlorination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The isolation at -78°C and characterization of the novel crystalline reactive porphinatomanganese(IV) complex Mn-(TDCPP)(OCl)2 (5) is described. 5 is compared with the porphinatomanganese(IV) complexes Mn(TDCPP)(C6H5IOCl)2 (2), Mn(TDCPP)(C6F510C1)CI (3) and Mn(TDCPP)(OCH3)2, (4). The stoichiometric reaction of 5 with triphenylphosphane yields 2.5 equivalents of triphenylphosphane oxide and 1.0 equivalent of Mn(TDCPP)Cl (1). Complex 5 epoxidizes stilbene, and oxygenates and chlorinates cyclohexane.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1135-1139 
    ISSN: 0009-2940
    Keywords: Arene complexes ; Chromium ; Allenes ; Rearrangements ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Cr(CO)3-complexed η6-phenylpropargylic alcohols 3 react in a displacement rearrangement with thionyl chloride or chlorodiphenylphosphane to give the chloro- or phosphoryl allenyl substituted η6-phenyl complexes 4 and 6, respectively. In the X-ray crystal structure of the novel organometallic allenic derivatives 4b and 6b the vicinal chloro or phosphoryl substituent and the benzene(tricarbonyl)chromium fragment are arranged coplanarily. Palladium/copper-catalyzed couplings of the chloroallene 4b with terminal alkynes disclose a facile access to ynallene derivatives 8, novel carbon-rich organometallic π-systems.
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