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  • Inorganic Chemistry  (92)
  • Wiley-Blackwell  (92)
  • American Meteorological Society
  • 1995-1999  (92)
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  • Wiley-Blackwell  (92)
  • American Meteorological Society
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  • 1
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1047-1052 
    ISSN: 0044-2313
    Schlagwort(e): Zirconium fluoride ; hafnium fluoride ; ternary fluorides ; KPdMIVF7 (MIV = Zr, Hf) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: 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).
    Notizen: 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).
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 2
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 993-1000 
    ISSN: 0044-2313
    Schlagwort(e): Zirconium(IV) fluoride ; hafnium(IV) fluoride ; Cs2Cu3MIVF12 (MIV = Zr, Hf) ; crystal structure ; magnetic properties ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: 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.
    Notizen: 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.
    Zusätzliches Material: 8 Ill.
    Materialart: Digitale Medien
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  • 3
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1227-1231 
    ISSN: 0044-2313
    Schlagwort(e): TiF4 ; preparation, single crystal structure ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: 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.
    Notizen: 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).
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 4
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1385-1394 
    ISSN: 0044-2313
    Schlagwort(e): Palladium ; quaternary fluorides ; LiPdGaF6 ; RbPdAlF6 ; K1.06Pd0.95Fe1.05F6 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: 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)].
    Notizen: 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).
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 5
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 99-103 
    ISSN: 0009-2940
    Schlagwort(e): Tri-tert-butylazadiboriridine ; (Hydroboryl)(methoxyboryl)amine ; 2,3-μ-Hydro-1,2,3-azoniadiborata-l-cyclopropenes ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The B—B bond of tri-tert-butylazadiboriridine [—NR—BR—BR—] (R = tBu; 1) is oxidized by MeOH to give the (hydroboryl)(methoxyboryl)amine H—BR=NR-BR(OMe) (2a). μ-2,3-Hydroazoniadiborata-1-cyclopropenes [=NR—BR(X)—μH—BR=] (3a, 3c-e) are formed by the action of the acids HX upon 1. A similar hydrogen bridge as in 3a-e is formed during the hydroboration of 1 by catecholborane, yielding 3f. A B atom is identified in the products 3a-f to be planarly coordinated by four atoms, two of which are forming a BHB three-center bond with that B atom. This is a novel bonding situation in boron chemistry. The structures of the products are deduced from 1H-, 11B-, and 13C-NMR spectra and are confirmed by X-ray structural analyses of 2a, 3a, and 3c.
    Zusätzliches Material: 2 Tab.
    Materialart: Digitale Medien
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  • 6
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 493-497 
    ISSN: 0009-2940
    Schlagwort(e): Organoaluminium compounds ; Alanes, 2-[(dimethylamino)methyl]phenyl- ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The reaction of LiAr (Ar = 2-[(dimethylamino)methyl]phenyl) with AlCl3, MeAlCl2, and Me2AlCl in a 1:1 ratio yields the corresponding organoaluminium compounds ArAlCl2, ArAl(Cl)Me, and ArAlMe2 (1-3). The alanes Ar2AlCl and Ar2AlMe (4 and 5) were synthesized from AlCl3 and MeAlCl2 with two equivalents of LiAr. The products ArAl(Cl)R [R = tBu, C(SiMe3)3] 6 and 7 are formed by the reaction of LiR with 1. The Lewis acid 1 adds the bases iPrNH2 and THF to yield the adducts 1 · iPrNH2 and 1 · THF. The structures of the products were deduced from the 1H-, 13C-, and 27Al-NMR spectra and were confirmed by X-ray structural determinations of 5 and 1 · iPrNH2.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 7
    ISSN: 0009-2940
    Schlagwort(e): Reductive silylation ; Aminochlorophosphanes ; Silylphosphanes ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 8
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 499-502 
    ISSN: 0009-2940
    Schlagwort(e): Phosphaalkenes ; Cycloadditions ; Insertion reactions ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 9
    ISSN: 0009-2940
    Schlagwort(e): Arene complexes ; Chromium compounds ; Substituent effects ; Push-pull chromophores ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The tricarbonylchromium complexes chlorobenzene 1 reacts with terminal alkynes 2 through a palladium-copper-catalyzed coupling to give a variety of Cr(CO)3-complexed phenylethynyl arenes, heteroarenes and ferrocene 3 in good to excellent yield. Due to the electron-withdrawing nature of the Cr(CO)3 group these novel complexes can be regarded as organometallic push-pull chromophores. Analogously, the corresponding free ligands 4 (phenylethynyl arenes, heteroarenes and ferrocene) were synthesized by coupling iodobenzene and 2. The crystal structure analysis of the singly Cr(CO)3-complexed tolane 3e reveals a strong deviation from coplanarity of both phenyl rings by an angle of 50.9(2)° presumably due to crystal packing. Correlations are established between selected substituent parameters (σP, σI, σR, σP+ and Δπ) and the carbonyl carbon resonances in the 13C-NMR spectra for the complexes 3. The overall electronic substituent effect is transmitted to the carbonyl groups by both mesomeric and inductive mechanisms. The push-pull complexes 3 display relatively small negative solvochromicities of longest wavelength absorption band (MLCT band).
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 10
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1579-1583 
    ISSN: 0009-2940
    Schlagwort(e): Silatetrazenes ; Nitrogen-silicon ring systems ; Bissilylamines ; Silicon-29 solid state NMR ; Aryl azides ; Chemistry ; Inorganic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The reaction between aryl azides and lithiated aryl amines leads to tetrazenes 3 and 9 which contain a chain of four nitrogen atoms. Reaction with different halosilanes gives the cyclic silatetrazenes 10, 12, and 15 where substitutents on the silicon vary form alkyl to hydrogen and chlorine atoms. The structures of 10, 12, and 15 in the solid state are reported. Variation of the solvent and the Lewis acidity of the halosilane influence the ratio of silatetrazene to side products, bissilyated amines. These effects are studied for different halosilanes.
    Zusätzliches Material: 2 Tab.
    Materialart: Digitale Medien
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