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  • Articles  (5)
  • Crystal Structure  (2)
  • X-ray structure analysis  (2)
  • CoII complex  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Zur Reaktion von Makrozyklen mit Lanthanoiden. II. Die Strukturen von [K(thf)3]2[(C22H28N4)2Sm2] · 4THF und [(C22H22N4)Co] · DME (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 81-85 
    Details
    ISSN: 0044-2313
    Keywords: SmIII polynuclear complex ; CoII complex ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reaction of Macrocycles with Lanthanoids. II. The Crystal Structures of [K(thf)3]2[(C22H28N4)2Sm2] · 4 THF and [(C22H22N4)Co] · DMEIn a complicated redox reaction [(TMTAA)K2] and [SmI2(thf)2] form the polynuclear metal complex [K(thf)3]2[(TMTAT)2Sm2]. This complex crystallizes with four molecules THF per formula unit and its structure was determined by single crystal X-ray investigation (spacegroup P21/c (No. 14), z = 4, a = 998.0(2) pm, = b = 2618.3(6) pm, c = 1619.4(3) pm, β = 96.52(2)°). In the dimeric unit [(TMTAT)2Sm2]2- the Sm3+ ions are bonded to the four N atoms of the macrocyclic ligand and one C6H4 ring of the second ligand is attached η6 like to one metal ion. Additionally two [K(thf)3]+ fragments are bonded to this central unit, and therefor coordination number seven results for the K+ ion. [TMTAA]2- is not reduced by [Cp2Co] in a similar reaction. The monomeric paramagnetic complex [(TMTAA)Co] (μeff = 2,76 μB) is formed instead. The structure reveils a square planar coordination of the Co atom by the four N atoms of the TMTAA ligand (spacegroup C2/c (No. 15), z = 4, a = 1945.1(4) pm, b = 1165.6(2) pm, c = 1144.7(2) pm, β = 116.38(1)°).
    Notes: [(TMTAA)K2] und [SmI2(thf)2] reagieren in einer unübersichtlichen Redoxreaktion zu dem mehrkernigen Metallkomplex [K(thf)3]2[(TMTAT)2Sm2]. Der Aufbau dieser mit vier Molekülen THF pro Formeleinheit kristallisierenden Verbindung konnte durch eine Röntgenstrukturanalyse aufgeklärt werden (Raumgruppe P21/c (Nr. 14), Z = 4, a = 998,0(2) pm, b = 2618,3(6) pm, c = 1619,4(3) pm, β = 96,52(2)°). In der dimeren Einheit [(TMTAT)2Sm2]2- sind die Sm3+-Ionen außer an die vier N-Atome eines makrozyklischen Liganden auch η6-artig an einen C6H4-Ring des zweiten Liganden gebunden. Zusätzlich koordinieren an die zentrale Einheit zwei [K(thf)3]+-Fragmente. Dies führt zu einer Koordinationszahl von 7 für das K+-Ion. [TMTAA]2- wird in einer analogen Reaktion mit [Cp2Co] nicht reduziert. Statt dessen bildet sich der monomere paramagnetische Komplex [(TMTAA)Co] (μeff = 2,76 μB). Nach der Kristallstrukturanalyse ist das Co-Atom quadratisch planar von den vier N-Atomen des TMTAA-Liganden koordiniert (Raumgruppe C2/c (Nr. 15), Z = 4, a = 1945,1(4) pm, b = 1165,6(2) pm, c = 1144,7(2) pm, β = 116,38(1)°).
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926150916
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  • 2
    Electronic Resource
    Electronic Resource
    Zur Reaktion von NiCl2 mit PhP(SiMe3)2 Die Kristallstruktur von [Ni12Cl2(PPh)2(P2Ph2)4(PHPh)8]Frau Professor Marianne Baudler zum 70. Geburtstage am 27. April 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 594 (1991), S. 29-35 
    Details
    ISSN: 0044-2313
    Keywords: Nickel(12) Cluster ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of NiCl2 with PhP(SiMe3)2, The Crystal Structure of [Ni12Cl2(PPh)2(P2Ph2)4(PHPh)8][Ni12Cl2(PPh)2(P2Ph2)4(PHPh)8] (1) has been prepared by the reaction of NiCl2 with PhP(SiMe3)2. The structure has been characterized by X-ray crystal structure analysis. 1 contains a Ni12-cluster with m̈4-PPh- and m̈6-P2Ph2- as bridging ligands. The terminal PHPh- and Cl-ligands are bound to Ni-atoms. The Ni12-cluster can be described as an Ni8-cube, in which four edges are bridged by Ni-atoms.
    Notes: NiCl2 und PhP(SiMe3)2 reagieren in THF unter Bildung von [Ni12Cl2(PPh)2(P2Ph2)4(PHPh)8] (1). Die Verbindung bildet schwarze Kristalle, deren Struktur durch eine Kristallstrukturanalyse aufgeklärt werden konnte. Danach liegt ein Ni12-Cluster vor, der m̈4-PPh- und m̈6-P2Ph2-Brückenliganden enthält. Die terminalen PHPh- und Cl-Liganden sind zusätzlich an Ni gebunden. Der Ni12-Cluster kann von einem Ni8-Kubus abgeleitet werden, in dem vier Kanten von Ni-Atomen überbrückt werden.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19915940104
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  • 3
    Electronic Resource
    Electronic Resource
    Darstellung und Struktur von [Cp2MoHLi(thf)]3 · Toluol (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 945-947 
    Details
    ISSN: 0044-2313
    Keywords: Molybdenum(II) ; Mo—Li heterobimetallic complex ; synthesis ; X-ray structure analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of [Cp2MoHLi(thf)]3 · Toluene[Cp2MoHLi]4 reacts in THF/Toluene to the trimeric complex [Cp2MoHLi(thf)]3 · Toluene 1.The structure of 1 was characterized by X-ray single crystal structure analysis. Space group P63, Z = 2, a = 1459.5(9) pm, c = 1182.3(8) pm. The central unit is represented by a Mo3Li3-hexagon. Each Mo-Atom is surrounded by two Cp-Ligands. One THF-Molecule is coordinated to each Li-atom. The Hydrogen-Ligand could not be located by the single crystal structure analysis.
    Notes: [Cp2MoHLi]4 reagiert in THF/Toluol zu der trimeren Verbindung [Cp2MoHLi(thf)]3 · Toluol 1.Der Aufbau von 1 wurde durch eine Kristallstrukturanalyse geklärt: Raumgruppe P63, Z = 2, a = 1459,5(9) pm, c = 1182,3(8) pm. Die zentrale Einheit in 1 bildet ein Mo3Li3-Sechsring. An jedes Mo-Atom koordinieren zwei Cp-Liganden. Jeweils ein THF-Molekül koordiniert an ein Li-Atom.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210607
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  • 4
    Electronic Resource
    Electronic Resource
    Synthese und Struktur eines Molybdän-Gadolinium-Heterometall-Komplexes Die Struktur von [Li(thf)4]2[Cp2MoSGdBr4(thf)]2 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 819-821 
    Details
    ISSN: 0044-2313
    Keywords: MoIV ; GdIII ; Mo—Gd heterobimetallic complex ; X-ray structure analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and structure of a Molybdenum-Gadolinium Heterometallic Complex. The Structure of [Li(thf)4]2[Cp2MoSGdBr4(thf)]2[Cp2MoHLi] reacts in THF with S and GdBr3 to yield the tetranuclear heterobimetallic complex [Li(thf)4]2[Cp2MoSGdBr4(thf)]2. The bonding situation and the structure of this compound were characterized by X-ray structure analysis (space group P1 (No. 2), Z = 1, a = 10.845(2) Å, b = 12.166(2) Å, c = 15.881(2) Å, α = 101.74(2)°, β = 97.62(2)°, γ = 103.97(2)°). Each S atom of the central Mo2S2-ring is coordinated by a GdBr4(thf) fragment. Additionally each Mo atom is connected to two Cp ligands. This leads to a tetrahedral coordination of the Mo atoms and a octahedral coordination of the Gd ions.
    Notes: [Cp2MoHLi] reagiert in THF mit S und GdBr3 zu dem vierkernigen Heterometallkomplex [Li(thf)4]2[Cp2MoSGdBr4(thf)]2. Die Bindungsverhältnisse und der Aufbau dieser Verbindung konnten durch eine Kristallstrukturanalyse geklärt werden (Raumgruppe P1 (Nr. 2), Z = 1, a = 10,845(2) Å, b = 12,166(2) Å, c = 15,881(2) Å, α = 101,74(2), β = 97,62(2)°, γ = 103,97(2)°). An den zentralen Mo2S2-Vierring koordiniert ein GdBr4(thf)-Fragment, so daß jedes Gd-Ion an sechs Liganden gebunden ist. Zusätzlich ist jedes Mo-Atom von zwei Cp-Liganden umgeben und erhält dadurch die Koordinationszahl 4.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200511
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  • 5
    Electronic Resource
    Electronic Resource
    Phosphaniminato-Komplexe des Vanadiums Die Kristallstruktur von [V3Cl6(NPMe3)5+]2[V4O4Cl8(NPMe3)22-] ·; 6 CH3CNProfessor Dietrich Babel zum 65. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1218-1222 
    Details
    ISSN: 0044-2313
    Keywords: Phosphoraneiminato Complexes of Vanadium ; Synthesis ; IR spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphoraneiminato Complexes of Vanadium. The Crystal Structure of [V3Cl6(NPMe3)5+]2[V4O4Cl8(NPMe3)22-] · 6 CH3CNVanadiumtetrachloride reacts in CCl4 solution with Me3SiNPMe3 to form the donor acceptor complex [VCl4(Me3SiNPMe3)], which reacts with excess Me3SiNPMe3 in boiling acetonitrile to form the phosphoraneiminato complex [V3Cl6(NPMe3)5]+Cl-. Partial hydrolysis in acetonitrile solution leads to black single crystals of [V3Cl6(NPMe3)5+]2[V4O4Cl8(NPMe3)22-] · 6 CH3CN, which are characterized by a crystal structure determination. Space group P21/c, Z = 2, structure solution with 3 008 observed unique reflections, R = 0.090. Lattice dimensions at -70°C: a = 1 379.0, b = 1 915.8, c = 2 278 pm, β = 102,79°. In the complex cation the three vanadium atoms form a trigonal bipyramid with two μ3-NPMe3 groups; the residual NPMe3- groups and the chlorine atoms are in terminal functions. In the anion [V4O4Cl8(NPMe3)2]2- the vanadium atoms are linked by μ2-O atoms to form a rectangle; in addition the two phosphoraneiminato ligands form μ2-N bridges.
    Notes: Vanadiumtetrachlorid reagiert in CCl4-Lösung mit Me3SiNPMe3 unter Bildung des Donor-Akzeptorkomplexes [VCl4(Me3SiNPMe3)], der sich in siedendem Acetonitril mit weiterem Me3SiNPMe3 zu dem Phosphaniminatokomplex [V3Cl6(NPMe3)5]+Cl- umsetzt. Durch partielle Hydrolyse in Acetonitrillösung entstehen hieraus schwarze Einkristalle [V3Cl6(NPMe3)5+]2[V4O4Cl8(NPMe3)22-] · 6 CH3CN, die wir röntgenographisch charakterisiert haben. Raumgruppe P21/c, Z = 2, Strukturlösung mit 3 008 unabhängigen beobachteten Reflexen, R = 0,090. Gitterkonstanten bei -70°C: a = 1 379,0; b = 1 915,8; c = 2 278 pm, β = 102,79°. In dem komplexen Kation bilden die drei Vanadiumatome mit zwei μ3-NPMe3-Gruppen eine trigonale Bipyramide, die drei übrigen NPMe3-Gruppen und die Chloratome sind terminal gebunden. In dem Anion [V4O4Cl8(NPMe3)2]2- sind die Vanadiumatome über μ2-O-Atome zu einem Rechteck verknüpft; zusätzlich fungieren die beiden Phosphaniminatoliganden als μ2-N-Brücken.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210718
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