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  • Inorganic Chemistry  (12)
  • (tBu2P)2P—SiMe3  (1)
  • 1H, 31P, 7Li-NMR spectra  (1)
  • Li(THF)2[η2-(Et2N)2P—P—PtBu2]  (1)
  • 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 Organo Transition Metal Compounds. 55. Preparation and Properties of Niobocenium and Tantalocenium Salts  -  Crystal and Molecular Structure of [(C5H5)2NbCl2][BF4] · CH3CNNiobocenium and tantalocenium compounds of the type [(C5H5)2MCl2]X (X = BF4, PBh4, PF6) were synthesized from the metallocene dichlorides and ferricenium salts, [(C5H5)2Fe]X, in methylene dichloride or tetrahydrofuran. With acetonitrile as solvent [(C5H5)2MCl2]X · CH3CN complexes are formed. Stable methyl compounds of the type [(C5H5)2M(CH3)2]X were obtained, when (C5H5)2Ta(CH3)2 is oxidized by means of ferricenium salts. The new complexes were characterized by elemental analysis, i. r., and 1H n.m.r. spectra. The structure of [(C5H5)2NbCl2][BF4] · CH3CN has been determined by X-ray structure analysis. The compound crystallizes in the orthorhombic space group Cmcm with a = 8.324(12), b = 19.581(13), c = 9,563(8) Å and Z = 4. The coordination geometry of the Nb atom is tetrahedrally.
    Notes: Niobocenium- und Tantalocenium-Verbindungen des Typs [(C5H5)2MCl2]X (X = BF4, PF6, BPh4) wurden aus den Metallocendichloriden und Ferricenium-Salzen, [(C5H5)2Fe]X, in Methylenchlorid bzw. Tetrahydrofuran als Reaktionsmedium erhalten. Bei Verwendung von Acetonitril entstanden Verbindungen des Typs [(C5H5)2MCl2]X · CH3CN (X = BF4, PF6). Durch Oxydation von (C5H5)2Ta(CH3)2 mit Ferricenium-Salzen waren stabile Komplexe der Zusammensetzung [(C5H5)2Ta(CH3)2]X zugängig.  -  Die dargestellten Verbindungen wurden charakterisiert durch Elementaranalysen sowie IR- und 1H-NMR-Spektren. Die Struktur der Verbindung [(C5H5)2NbCl2][BF4] · CH3CN wurde durch Röntgenkristallstrukturanalyse bestimmt. Die Verbindung kristallisiert orthorhombisch in der Raumgruppe Cmcm mit den Gitterkonstanten a = 8,324(12), b = 19,581(13), c = 9,563(8) Å und Z = 4. Die Koordinationsgeometrie des Nb-Atoms ist tetraedrisch.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 605 (1991), S. 109-116 
    ISSN: 0044-2313
    Keywords: Antimony(III)fluoride,(Sb2F5+)(Sb3F72+)(SbF6-)3 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of a new Modification of Sb8F30The modification of Sb8F30, described here, crystallizes in the orthorhombic space group Pca21 (No. 29) with a = 1115.7(1), b = 1100.2(1), c = 1917.8(3) pm and Z = 4. Within this complex molecule, the Sb3F72+-cation was identified besides a heavily distorted form of the mixed valent Sb4F17--anion.
    Notes: Die hier beschriebene Modifikation von Sb8F30 kristallisiert in der orthorhombischen Raumgruppe Pca21 (Nr. 29) mit a = 1115,7(1), b = 1100,2(1), c = 1917,8(3) pm und Z = 4. Innerhalb dieses komplexen Moleküls werden ein Sb3F72+-Kation und eine stark verzerrte Form des gemischt valenten Sb4F17--Anions identifiziert.
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  • 3
    ISSN: 0044-2313
    Keywords: Bis[triglymesodium(1+)][Tetrakis(borane)sulfate(2-)], [Na · Triglyme]2[S(BH3)4] ; preparation ; crystal structure ; SCF calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Na · Triglyme]2[S(BH3)4]: a Salt of the New Anion Tetrakis(borane)sulfate(2- ). Crystal Structure and Theoretical Investigation of the StructureNa[H3B-m̈2-S(B2H5)] 1 is produced by the reaction between NaSH and THF · BH3, under dehydrogenation. 1 is also formed as the first 11B-NMR-spectroscopically detectable reaction product by the reaction between anhydrous Na2S and THF · BH3. Adducts of BH3 with the S2- ion are not detectable in THF. The anion [S(BH3)4]2- can however be obtained, by the addition of NaBH4 to 1 in diglyme or triglyme respectively: [Na  -  Triglyme]2[S(BH3)4] 2. 2 crystallizes in the monoclinic space group P21/n (Nr. 14). Structural data of 1 and 2 have been calculated by SCF methods. The anion of 2 may be viewed either as an adduct of B2H6 with S2-, or as a bridge substituted thia derivative of B2H7-; furthermore the anion of 2 is isoelectronic and isostructural with the SO42- ion.
    Notes: Bei der Reaktion zwischen NaSH und THF · BH3 entsteht unter H2-Abspaltung Na[H3B-m̈2-S(B2H5)] 1. 1 entsteht auch als erstes 11B-NMR-spektroskopisch nachweisbares Reaktionsprodukt bei der Reaktion zwischen wasserfreiem Na2S und THF · BH3. Addukte von BH3 an das S2--Ion lassen sich in THF als Lösungsmittel nicht nachweisen. Das neue Anion [S(BH3)4]2- kann jedoch durch Addition von NaBH4 an 1 in Diglyme bzw. Triglyme erhalten werden: [Na · L]2[S(BH3)4] 2. 2 kristallisiert monoklin in der Raumgruppe P21/n (Nr. 14). Aus SCF-Rechnungen erhielten wir die Strukturparameter für 1 und 2. Das Anion von 2 kann sowohl als Addukt von B2H6 an S2- als auch als brückensubstituiertes Thia-Derivat des B2H7--Ions aufgefaßt werden; ferner ist es isoelektronisch und isostrukturell mit dem SO42-- Ion.
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  • 4
    ISSN: 0044-2313
    Keywords: Copper Molybdate ; Phase Investigation ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure and Properties of CuxMoO3Cu0.185MoO3 was found in the coexistence range MoO3—Cu4Mo5O17—MoO2. The structure was determined by X-ray diffraction on selected monocrystals. The compound crystallizes in the monoclinic space group C2/c (a = 1 668.8(3), b = 932.2(3), c = 543.1(2) pm, β = 102,78(1)°, Z = 2).
    Notes: Cu0,185MoO3 wurde im Koexistenzgebiet MoO3—Cu4Mo5O17—MoO2 nachgewiesen. Die Strukturbestimmung erfolgte durch Röntgenbeugung an ausgelesenen Einkristallen. Cu0,185MoO3 kristallisiert in der monoklinen Raumgruppe C2/c (a = 1 668,8(3), b = 932,2(3), c = 543,1(2) pm, β = 102,78(1)°, Z = 2).
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  • 5
    ISSN: 0044-2313
    Keywords: Li(THF)2[η2-(tBu2P)2P] ; Li(TMEDA)[η2-(tBu2P)2P] ; Li(THF)2[η2-(iPr2P)2P] ; Li(THF)2[η2-(Et2N)2P—P—PtBu2] ; Li(THF)2[η2-(tBu2P—P—PiPr2)] ; (tBu2P)2P—SiMe3 ; crystal structures ; 1H, 31P, 7Li-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation and Structure of Li(THF)2[η2-(tBu2P)2P], Li(TMEDA)[η2-(tBu2P)2P], Li(THF)2[η2-(iPr2P)2P], Li(THF)2[η2-(Et2N)2P—P—PtBu2], Li(THF)2[η2-(tBu2P—P—PiPr2] and (tBu2P)2P—SiMe3The formation and crystal structures of the compounds (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA)[η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 and Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 are reported. Compounds 3-6 are formed by reacting the corresponding silylated triphosphanes with nBuLi: 2 and 3 result from (tBu2P)2P—SiMe3 1, 4 from (iPrP)2P—SiMe3, 5 from (Et2N)2P—P(SiMe3)—PtBu2 and 6 from tBu2P—P(SiMe3)—PiPr2. 1 crystallizes in the orthorhombic space group P212121 (no. 19) with a = 910.87(7) pm, b = 1132.5(1) pm, c = 2373.5(2) pm (determined at 90 K). The structure determination of 2 was performed at 293 K and 200 K, respectively. 2 crystallizes in the monoclinic space group P21/n (no. 14) with a = 1069.7(3) pm, b = 1802.5(3) pm, c = 1604.0(7) pm, β = 98.11(2)° (200 K); 3 also in P21/n (no. 14) with a = 904.3(2) pm, b = 1936.4(5) pm, c = 1653.2(3) pm, β = 94.52(1)° (200 K). 4 crystallizes monoclinically in C2/c (no. 15) with a = 1650.0(5) pm, b = 945.6(3) pm, c = 1779.8(5) pm, β = 108.81(2)° (200 K); 5 in P21/n (no. 14) with a = 939.4(5) pm, b = 1736.8(6) pm, c = 1943.3(7) pm, β = 98.17(4)° (200 K). All compounds contain Z = 4 molecules in the unit cell.The 1H, 31P and 7Li NMR spectra of 2-6 are discussed.
    Notes: Es wird über die Verbindungen (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA) · [η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 und Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 berichtet. Letztere bilden sich durch Umsetzung der entsprechenden silylierten Triphosphane mit nBuLi: 2 und 3 aus (tBu2P)2P—SiMe3 1, 4 aus (iPr2P)2P—SiMe3, 5 aus (Et2N)2—P · (SiMe3)—PtBu2, 6 aus tBu2P—P(SiMe3)—PiPr2.1 kristallisiert orthorhombisch in P212121 (Nr. 19) mit a = 910,87(7) pm, b = 1132,5(1) pm, c = 2373,5(2) pm (bei 90 K bestimmt). Die Strukturbestimmung von 2 erfolgte bei 293 K und 200 K. 2 kristallisiert monoklin in P21/n (Nr. 14) mit a = 1069,7(3) pm, b = 1802,5(3) pm, c = 1604,0(7) pm, β = 98,11(2)° (200 K), 3 ebenfalls in P21/n (Nr. 14) mit a = 904,3(2) pm, b = 1936,4(5) pm, c = 1653,2(3) pm, β = 94,52(1)° (200 K). 4 kristallisiert monoklin in C2/c (Nr. 15) mit a = 1650,0(5) pm, b = 945,6(3) pm, c = 1779,8(5) pm, β = 108,81(2)° (200K), 5 in P21/n (Nr. 14) mit a = 939,4(5) pm, b = 1736,8(6) pm, c = 1943,3(7) pm, β = 98,17(4)° (200 K). Alle fünf Verbindungen enthalten jeweils vier Formeleinheiten in der Elementarzelle.Es wird über die Untersuchung der 1H-, 31P- und 7Li-NMR-Spektren der Verbindungen 2-6 berichtet.
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  • 6
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation of CH3SCN · MF5 Adducts (M = As, Sb) and Crystal Structure of CH3SCN · AsF5The preparation and spectroscopic characterization of CH3SCN · MF5 M = As, Sb is reported. X-Ray structure analysis shows that the adduct CH3SCN · AsF5 is N coordinated. It crystallizes in the monoclinic space group P21/m (Nr. 11) with a = 537.07(6) pm, b = 755.28(10) pm, c = 863.19(10) pm, β = 91.81(1)°, Z = 2. The geometric parameters correspond to the expected values.
    Notes: Es wird über die Darstellung von CH3SCN · MF5 (M = As, Sb) und ihre spektroskopische Charakterisierung berichtet. Nach einer Strukturanalyse durch Röntgenbeugung ist das Addukt CH3SCN · AsF5 über N koordiniert und kristallisiert in der monoklinen Raumgruppe P21/m (Nr. 11) mit a = 537,07(6) pm, b = 755,28(10) pm, c = 863,19(10) pm, β = 91,81(1)°, und Z = 2. Die Geometrieparameter entsprechen den Erwartungen.
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  • 7
    ISSN: 0044-2313
    Keywords: Oxomolybdates ; X-Ray Crystal Structure ; Twinning ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of Two Forms of In5Mo18O28 and TwinningIn5Mo18O28 is prepared from In, Mo and MoO2 at 1 150°C in an evacuated quartz glass ampoule. X-ray investigations on single crystals show monoclinic symmetry (a = 1 323.13(9), b = 951.88(10), c = 989.48(8) pm, β = 100.976(4)°, space group P 21/c (No. 14)) for form 1. The second form (2) crystallizes in the orthorhombic system (space group Pmcn (No. 62), a = 2 596.6(5), b = 952.0(2), c = 989.6(2) pm). Twinning and charge balances are discussed.
    Notes: Beim Tempern von Indium mit Molybdän und Molybdändioxid in verschlossenen Quarzglasampullen bei 1 150°C erhält man die Verbindung In5Mo18O28. Untersuchungen an Einkristallen ergeben für die Modifikation 1 eine monokline Struktur (a = 1 323,13(9), b = 951,88(10), c = 989,48(8) pm, β = 100,976(4)°, Raumgruppe P 21/c (Nr. 14)). Die zweite Modifikation (2) kristallisiert orthorhombisch in der Raumgruppe Pmcn (Nr. 62, a = 2 596,6(5), b = 952,0(2), c = 989,6(2) pm). Zwillingsbildung und Ladungsbilanzen werden diskutiert.
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  • 8
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorus(III) Thiohalides: Sd=P—F and S=P—Br. Mass Spectrometric InvestigationsThe compounds S=P—F and S=P—Br are formed by reaction of P(S)FBr2 and P(S)Br3, respectively, with silver at temperatures of about 800 K. S=P—Br is also formed by pyrolysis of P(S)Br3 at temperatures above 298 K. Mass spectrometric equilibrium measurements lead to the heat of formation of S=P—F: ΔH°298(SPFg) = -260.8 kJ/mol.
    Notes: Die Homologen der Thiazylhalogenide, S=P—F und S=P—Br, entstehen bei ber Reduktion von P(S)FBr2 bzw. P(S)Br3 mit elementarem Silber bei Temperaturen um 800 K. Zu S=P—Br gelangt man ebenfalls durch Thermolyse von P(S)Br3 bei Temperaturen wenig oberhalb Zimmertemperatur. Aus massenspektrometrischen Untersuchungen der Gleichgewichtslage wurde für S=P—F eine Bildungsenthalpie von -260,8 kJ/mol abgeleitet.
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  • 9
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fluoro Substituted and other New CarbodiphosphoranesSyntheses and properties of the carbodiphosphoranes [(CH3)2N]3P=C=P(CH3)[N(CH3) 2]2, (3), [(CH3)2N]2(F)P=C=P(F) [N(CH3)2]2, (7), and (C6H5)2(F)P=C=P(F)(C6H5) 2, (11), are discribed. The compounds 3, 7, and 11 as well as [(C2H5)2N]3P=C=P(CH3) [(C2H5)2N]2 are characterized by their 1H, 13C, 19F, and 31P n.m.r. and mass spectra. The crystal and molecular structures of 7 are reported.
    Notes: Synthese und Eigenschaften der Carbodiphosphorane [(CH3)2N]3P=C=P(CH3)[N(CH3)2]2, (3), [(CH3)2N]2(F)P=C=P(F)[N(CH3)2]2, (7), und (C6H5)2(F)P=C=P(F)(C6H5) 2, (11), werden beschrieben. Die Verbindungen 3, 7 und 11 sowie [(C2H5)2N]3P=C= P(CH3)[(C2H5)2N]2 sind durch ihre 1H-, 13C-, 19F- und 31P-NMR-Spektren sowie durch ihre Massenspektren charakterisiert. Die Kristall- und Molekülstruktur von 7 werden mitgeteilt.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 93-98 
    ISSN: 0044-2313
    Keywords: Tetrachloroarsonium(V) ; Hexafluoroarsenate(V) ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Redetermination of the Crystal Structure of AsCl4+AsF6-The X-ray crystal structure analysis of AsCl4+AsF6- (P4/n (Nr. 85), a = b = 866.65(15) pm, c = 623.78(17) pm, Z = 2) is reported. Some structural parameters differ largely from values obtained by Weissenberg pictures.
    Notes: Es wird über die Kristallstruktur von AsCl4+AsF6- (P4/n (Nr. 85) a = b = 866,65(15) pm, c = 623,78(17) pm, Z = 2) berichtet. Einige Strukturparameter unterscheiden sich erheblich von früheren aus Weissenberg-Aufnahmen bestimmten Werten.
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