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  • 1
    ISSN: 0044-2313
    Keywords: Non-oxo Vanadium(IV) Complexes ; Mass Spectra ; Cyclovoltammetry ; Bis[2,2′-dihydroxy-azobenzenato(2)]vanadium(IV) ; Trigonal-prismatic Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Non-oxo Vanadium(IV) Complexes with Tridentate Diacidic Ligands. Molecular Structure of Bis[2.2′-dihydroxy-azobenzenato(2-)]vanadium(IV)By the reaction of tris(acetylacetonato)vanadium(III) with tridentate diacidic ligands non-oxo vanadium(IV) complexes of these ligands were synthesized. The complexes were characterized by mass spectrometry. Electrochemical studies show that the complexes are reversibly oxidized or reduced. Bis[2,2′-dihydroxy-azobenzenato(2-)]vanadium(IV) has a distorted trigonal-prismatic structure. Crystallographic data see „Inhaltsübersicht“.
    Notes: Durch Reaktion von Tris(acetylacetonato)-vanadium(III) mit dreizähnigen diaciden Liganden wurden oxofreie Vanadium(IV)-Komplexe dieser Liganden dargestellt. Die Komplexe wurden massenspektrometrisch charakterisiert. Sie können elektrochemisch reversibel oxidiert und reduziert werden. Bis[2,2′-dihydroxy-azobenzenato(2-)]vanadium(IV) besitzt eine verzerrt trigonal-prismatische Struktur. Raumgruppe P21/n, Z = 4, 1 812 beobachtete unabhängige Reflexe, R = 5,9%. Gitterabmessungen bei 19°C; a = 9,973(2) pm, b = 15,435(3) pm, c = 13,763(3) pm, β = 104,79(3)°.
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  • 2
    ISSN: 0044-2313
    Keywords: Antimony(V)-oxide chloride ; Synthesis ; IR Spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, IR Spectrum, and Crystal Structure of Sb12O18(OH)2Cl22 · 2CH2Cl2The title compound has been prepared by the reaction of Sb5O7Cl11 with dichloromethane at 20°C, forming colourless, moisture sensitive crystals. Sb12O18(OH)2Cl22 · 2CH2Cl2 crystallizes monoclinically in the space group P21/n with two formula units per unit cell. Structure solution with 2696 unique observed reflections, R = 0.042. Lattice dimensions at 19°C: a = 1350.2, b = 1466.7, c = 1392.9 pm, b̃ = 97.925°. The distorted octahedrally coordinated antimony atoms, bridged by oxygen atoms, exhibit a molecular array which may be seen as a fragment of the rutile type structure, isolated by terminal chloride ligands. The solvate molecule is associated by a hydrogen bridge OH···Cl.
    Notes: Die Titelverbindung entsteht in Form farbloser Kristalle bei der Reaktion von Sb5O7Cl11 mit Dichlormethan bei 20°C. Sb12O18(OH)2Cl22 · 2CH2Cl2 kristallisiert monoklin in der Raumgruppe P21/n mit zwei Formeleinheiten pro Elementarzelle. Strukturlösung mit 2696 unabhängigen beobachteten Reflexen, R = 0,042. Gitterkonstanten bei 19°C: a = 1350,2; b = 1466,7; c = 1392,9 pm, b̃ = 97,925°. Die verzerrt oktaedrisch koordinierten und über Sauerstoffatome verbrückten Antimonatome bilden ein molekulares Gerüst, das als ein durch terminale Chlorliganden isolierter Ausschnitt aus der Rutilstruktur angesehen werden kann. Das Solvatmolekül ist durch eine Wasserstoffbrücke OH…Cl assoziiert.
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  • 3
    ISSN: 0044-2313
    Keywords: Dioxomolybdenum(VI) complexes ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ligand Exchange Reactions of Bis(acetylacetonato)dioxo-molybdenum(VI). Crystal Structures of [Salicylaldehyde-benzoylhydrazonato(2-)]dioxo-methanol-molybdenum(VI) and [Benzoylacetone-benzoylhydrazonato(2-)]dioxo-triphenylphosphaneoxide-molybdenum(VI)The products of ligand exchange reactions between bis(acetylacetonato)dioxo-molybdenum(VI) and tridentate diacidic ligands H2L in the presence of triphenylphosphane were found by mass spectrometry to be complexes of the type MoO2L. In the case of salicylaldehyde 2-hydroxyanil MoL2 could also be identified. The compounds MoO2L were crystallized as complexes with methanol or triphenylphosphane oxide.Crystallographic data see “Inhaltsübersicht”.
    Notes: Als Reaktionsprodukte bei der Ligandenaustauschreaktion von Bis(acetylacetonato)dioxo-molybdän(VI) mit dreizähnigen diaciden Liganden H2L in Gegenwart von Triphenylphosphan wurden massenspektrometrisch Komplexe des Typs MoO2L identifiziert. Beim Salicylaldehyd-2-hydroxyanil konnte auch MoL2 nachgewiesen werden. Die Verbindungen MoO2L kristallisieren als Komplexe mit Methanol oder Triphenylphosphanoxid.[Salicylaldehyd-benzoylhydrazonato-(2-)]dioxo-methanol-molybdän(VI): Raumgruppe P1, Z = 2, 3 073 unabhängige Reflexe, R = 3,2%; Gitterabmessungen bei 19°C: a = 785,5(2) pm, b = 980,6(2) pm, c = 1 037,2(2) pm, α = 94,53(3)°, β = 107,38(3)°, γ = 90,35(3)°, [Benzoylaceton-benzoylhydrazonato(2-)]dioxo-triphenylphosphanoxid-molybdän(VI); Raumgruppe P21/n, Z = 4, 8 147 unabhängige Reflexe, R = 3,55% Gitterabmessungen bei 20°C: a = 1 091,3(2) pm, b = 1 512,8(3) pm, c = 1897,1(4) pm, β = 92,25(3)°.
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  • 4
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes of Titanium, Synthesis, Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorane Iminato Complexes of Titanium. The Crystal Structures of [TiCl2(NPPh3)2] and [TiCl3(NPMe2Ph)(CH3CN)]2[TiCl2(NPPh3)2] has been prepared by the reaction of [TiCl3(NPPh3)] with excess Me3SiNPPh3 in a melt at 220°C, forming colourless crystals. [TiCl3(NPMe2Ph)(CH3CN)]2 is formed as yellow, moisture sensitive crystals from acetontrile solutions of [TiCl3(NPMe2Ph)]2, which on its part has been obtained by the reaction of TiCl4 with Me3SiNPMe2Ph. The complexes are characterized by IR spectroscopy and by crystal structure determinations.[TiCl2(NPPh3)2]. Space group Fdd2, Z = 8, structure refinement with 2875 observed unique reflections, R = 0.039. Lattice dimensions at 19°C: a = 2080.9, b = 3308.5, c = 973.6 pm. The compound forms monomeric molecules with bond lengths TiN of 179.0 pm and PN of 156.8 pm, which correspond with double bonds. The bond angle TiNP is 166.6°.[TiCl3(NPMe2Ph)(CH3CN)]2. Space group P1, Z = 1, structure refinement with 2577 unique reflections, R = 0.039 for reflections with I 〉 2σ(I). Lattice dimensions at 20°C: a = 856.6, b = 923.1, c = 1008.3 pm, α = 81.23°, β = 71.63°, γ = 81.41°. The compound forms centrosymmetric, dimeric molecules, in which the titanium atoms are linked via chloro bridges TiCl2Ti with TiCl bond lengths of 243.9 and 270.3 pm. In trans-position to the longer TiCl bonds the nitrogen atoms of the phosphorane iminato groups are coordinated with bond lengths TiN of 173.9 pm and PN of 161.4 pm which again correspond with double bonds. The bond angle TiNP is 156.4°.
    Notes: [TiCl2(NPPh3)2] wird in Form farbloser Kristalle durch Schmelzreaktion von [TiCl3(NPPh3)] mit überschüssigem Me3SiNPPh3 bei 220°C erhalten. [TiCl3(NPMe2Ph) · (CH3CN)]2 bildet gelbe, feuchtigkeitsempfindliche Kristalle, die aus Acetonitrillösung von [TiCl3(NPMe2Ph)]2 erhalten werden, welches seinerseits aus TiCl4 und Me3SiNPMe2Ph entsteht. Die Komplexe werden durch ihre IR-Spektren und durch Kristallstrukturanalysen charakterisiert.[TiCl2(NPPh3)2]. Raumgruppe Fdd2, Z = 8, Strukturverfeinerung mit 2875 beobachteten unabhängigen Reflexen, R = 0,039. Gitterabmessungen bei 19°C: a = 2080,9; b = 3308,5; c = 973,6 pm. Die Verbindung bildet monomere Moleküle mit Abständen TiN von 179,0 pm und PN von 156,8 pm, die Doppelbindungen entsprechen, und einem TiNP-Bindungswinkel von 166,6°.[TiCl3(NPMe2Ph)(CH3CN)]2. Raumgruppe P1, Z = 1, Strukturverfeinerung mit 2577 unabhängigen Reflexen, R = 0,039 für Reflexe mit I 〉 2σ(I). Gitterabmessungen bei 20°C: a = 856,6; b = 923,1; c = 1008,3 pm, α = 81,23°; β = 71,63°; γ = 81,41°. Die Verbindung bildet zentrosymmetrische, dimere Moleküle, in denen die Titanatome über TiCl2Ti-Brücken mit TiCl-Abständen von 243,9 und 270,3 pm verknüpft sind. In den trans-Positionen zu den langen Bindungen befinden sich die N-Atome der Phosphaniminatogruppen mit Abständen TiN von 173,9 pm und PN von 161,4 pm, die wiederum Doppelbindungen entsprechen. Der TiNP-Bindungswinkel beträgt 156,4°.
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  • 5
    ISSN: 0044-2313
    Keywords: Phosphoraneimine Complexes of Iodine Chlorides, Syntheses, IR Spectra, Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Silylated Phosphorane Imines with Iodine Monochloride and Iodine Trichloride. The Crystal Structures of [Me3SiNPMe3 · ICl], [Ph3PNCl · ICl], and [Me3PN(H)PMe3][ICl2]2The donor-acceptor complex [Me3SiNPMe3 · ICl] has been prepared from Me3SiNPMe3 and ICl in acetonitrile solution forming yellow-orange crystals. [Ph3PNCl · ICl] can be prepared by the reaction of Me3SiNPPh3 with ICl3 in dichloromethane solution forming pale yellow crystals. [Me3PN(H)PMe3][ICl2]2 is formed in a small amount by a slow reaction of Me3SiNPMe3 with ICl3 in CCl4 suspension in the presence of traces of moisture. All samples are characterized by IR spectroscopy and by X-ray structure analyses.[Me3SiNPMe3 · ICl] (1): Space group Iba2, Z = 8, structure solution with 1 727 observed unique reflections, R = 0.051. Lattice dimensions at -60°C: a = 1 510.7, b = 1 862.8, c = 988.9 pm. 1 has a molecular structure in which the N atom of the phosphorane imine is connected with the iodine atom of the ICl molecule in a linear arrangement N—I—Cl. Bond lengths N—I = 222.7 pm, I—Cl = 265.1 pm.[Ph3PNCl · ICl] (2): Space group Pna21, Z = 4, structure solution with 1 530 observed unique reflections, R = 0.030. Lattice dimensions at 20°C: a = 1 522.8, b = 1 408.3, c = 865.8 pm. 2 has a molecular structure in which the N atom of the N chlorophosphorane imine is connected with the iodine atom of the ICl molecule in a linear arrangement. Bond lengths N—Cl = 174.4 pm, N—I = 229.5 pm, I—Cl = 251.2 pm.[Me3PN(H)PMe3][ICl2]2 (3): Space group P21/c, Z = 4, structure solution with 1 989 observed unique reflections, R = 0.029. Lattice dimensions at -50°C: a = 1 223.1, b = 1 090.2, c = 1 482.8 pm, β = 112.21°. 3 consists of [Me3PN(H)PMe3]2+ ions and ICl2- anions. The PNP bond angle of the dication amounts to 134.4° with PN distances of 165.6 and 166.1 pm, approximately according to double bonds.
    Notes: Der Donor-Akzeptorkomplex [Me3SiNPMe3 · ICl] entsteht aus Me3SiNPMe3 und ICl in Acetonitrillösung als gelborange Kristalle. [Ph3PNCl ·ICl] wird durch Umsetzung von Me3SiNPPh3 mit ICl3 in Dichlormethanlösung als hellgelbe Kristalle erhalten. [Me3PN(H)PMe3][ICl2]2 bildet sich in geringer Menge aus Me3SiNPMe3 und ICl3 in Tetrachlorkohlenstoff nach Zutritt von Feuchtigkeit. Alle Präparate werden durch die IR-Spektren und durch Kristallstrukturanalysen charakterisiert.[Me3SiNPMe3 · ICl] (1): Raumgruppe Iba2, Z = 8, Strukturlösung mit 1 727 beobachteten unabhängigen Reflexen, R = 0,051. Gitterkonstanten bei -60°C: a = 1 510,7; b = 1 862,8; c = 988,9 pm. 1 hat eine Molekülstruktur, in der das N-Atom des Phosphanimins mit dem Iodatom des ICl-Moleküls in linearer Anordnung N—I—Cl verknüpft ist. Bindungslängen N—I = 222,7 pm, I—Cl = 265,1 pm.[Ph3PNCl · ICl] (2): Raumgruppe Pna21, Z = 4, Strukturlösung mit 1 530 beobachteten, unabhängigen Reflexen, R = 0,030. Gitterkonstanten bei 20°C: a = 1 522,8; b = 1 408,3; c = 865,8 pm. 2 hat eine Molekülstruktur, in der das N-Atom des N-Chlorphosphanimins mit dem Iodatom des ICl-Moleküls in linearer Anordnung verknüpft ist. Bindungslängen N—Cl = 174,4 pm, N—I = 229,5 pm, I—Cl = 251,2 pm.[Me3PN(H)PMe3][ICl2]2 (3): Raumgruppe P21/c, Z = 4, Strukturlösung mit 1 989 beobachteten unabhängigen Reflexen, R = 0,029. Gitterkonstanten bei -50°C: a = 1 223,1; b = 1 090,2; c = 1 482,8 pm, β = 112,21°. 3 besteht aus [Me3PN(H)PMe3]2+-Ionen und ICl2--Anionen. Der PNP-Bindungswinkel des Dikations beträgt 134,4° bei PN-Abständen von 165,6 und 166,1 pm, die etwa Doppelbindungen entsprechen.
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  • 6
    ISSN: 0044-2313
    Keywords: Non-oxo Vanadium(IV) Complex ; Bis[salicylaldehyde-2-hydroxyanilato(2 - )]vanadium(IV) ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Molecular Structure of Bis[salicylaldehyde-2-hydroxyanilato(2 - )]vanadium(IV)By the reaction of tris(acetylacetonato)vanadium(III) with salicylaldehyde-2-hydroxyanil the non-oxo vanadium(IV) complex of this ligand was prepared. Bis[salicylaldehyde-2-hydroxyanilato(2 - )]vanadium(IV) has a distorted octahedral structure. Crystallographic data see “Inhaltsübersicht”.
    Notes: Durch Reaktion von Tris(acetylacetonato)vanadium(III) mit Salicylaldehyd-2-hydroxyanil wurde der oxofreie Vanadium(IV)-Komplex dieses Liganden dargestellt und durch Röntgenkristallstrukturanalyse die Struktur bestimmt. Bis[salicylaldehyd-2-hydroxyanilato(2 - )]vanadium(IV) besitzt eine verzerrt-oktaedrische Struktur. Raumgruppe P1, Z = 4, 2722 beobachtete, symmetrieunabhängige Reflexe, R = 7,1%. Gitterabmessungen bei 293 K: a = 964,6(1) pm, b = 1285,4(1) pm, c = 1788,9(2) pm, α = 81,42(1)°, β = 74,39(1)°, γ = 89,33(1)°.
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  • 7
    Electronic Resource
    Electronic Resource
    Springer
    Naturwissenschaften 40 (1953), S. 17-18 
    ISSN: 1432-1904
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology , Natural Sciences in General
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  • 8
    Publication Date: 1953-01-01
    Print ISSN: 0028-1042
    Electronic ISSN: 1432-1904
    Topics: Biology , Chemistry and Pharmacology , Natural Sciences in General
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