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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 941-944 
    ISSN: 0044-2313
    Keywords: GdIII trigonal prismatic complexes ; 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 the Lanthanides with Chelate Ligands Synthesis and Crystal Structure of [(py2CH)3Gd]GdBr3 reacts with [(py2CH)Li] to the mononuclear complex [(py2CH)3Gd] 1.The structure of 1 was characterized by X-ray single crystal structure analysis. Space group P21, Z = 2, a = 951.4(10) pm, b = 1369.4(10) pm, c = 1074.5(10) pm, β = 105.69(8)°.The Gd-Ion is surrounded by the six nitrogen atoms of the three chelate ligands and shows a distorted trigonal prismatic coordination. As a difference to the lithium salt of the ligand, the six-membered metalla-cycles in 1 are not planar, but show a boat conformation.
    Notes: GdBr3 reagiert mit [(py2CH)Li] zu dem einkernigen Komplex [(py2CH)3Gd] 1.Der Aufbau von 1 wurde durch eine Kristallstrukturanalyse geklärt: Raumgruppe P21, Z = 2, a = 951,4(10) pm, b = 1369,4(10) pm, c = 1074,5(10) pm, β = 105,69(8)°.Das Gd-Ion ist von den sechs Stickstoff-Atomen der drei Chelatliganden koordiniert und besitzt eine verzerrt trigonalprismatische Umgebung. Die in 1 gebildeten Metalla-Sechsringe sind im Gegensatz zum Lithiumsalz des Liganden nicht planar, sondern zeigen Wannenkonformation.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 945-947 
    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.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 948-952 
    ISSN: 0044-2313
    Keywords: Gadolinium(III) ; Samarium(III) ; pentahedral complexes ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Results in the Chemistry of Lanthanoide Complexes. The Crystal Structures of [(C11H21N2)2LnBr] (Ln = Sm, Gd)LnBr3 leads with [(iPr2AIP)Li] (AIP = 2-iPropylamino-4-iPropylimino-2-Pentene) to the mononuclear complex [(iPr2AIP)2LnBr] (Ln = Gd 1, Sm = 2).The structures of 1-2 were characterized by X-ray single crystal structure analysis.1:Space group Cc, Z = 4, a = 1283.3(7) pm, b = 1558.6(8) pm, c = 1330.1(7) pm, β = 90.24(4)°2:Space group Cc, Z = 4, a = 1281.7(2) pm, b = 1562.3(3) pm, c = 1329.8(2) pm, β = 90.09(1)°.The Ln-Ion is coordinated by a Brom-Atom and the four Nitrogen-Atoms of the chelate ligand.
    Notes: LnBr3 reagiert mit [(iPr2AIP)Li] (AIP = 2-iPropylamino-4-iPropylimino-2-Penten) zu dem einkernigen Komplex [(iPr2AIP)2LnBr] (Ln = Gd 1, Sm 2).Der Aufbau von 1-2 konnte durch Kristallstrukturanalyse geklärt werden: 1:Raumgruppe Cc, Z = 4, a = 1283,3(7) pm, b = 1558,6(8) pm, c = 1330,1(7) pm, β = 90,24(4)°.2:Raumgruppe Cc, Z = 4, a = 1281,7(2) pm, b = 1562,3(3) pm, c = 1329,8(2) pm, β = 90,09(1)°. Das Ln-Ion ist durch ein Brom-Atom und die vier Stickstoff-Atome der zwei Chelatliganden fünffach koordiniert.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 77-80 
    ISSN: 0044-2313
    Keywords: CeIII double decker 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. I. The Crystal Structure of [Li(thf)][(C22H22N4)2Ce] · THFIn THF CeBr3 forms with [(TMTAA)Li2] the paramagnetic doubledecker complex [Li(thf)][(TMTAA)2Ce]. The complex crystallizes with 1 Mol THF per formula unit. The structure was characterized by X-ray single crystal structure analysis (space group C2 (No. 5), z = 6, a = 1741.8(2) pm, b = 1622.1(2) pm, c = 2540.4(3) pm, β = 104.72(1)°). The sandwich-like arrangement of the heterocyclic ligands leads to a quadratic-prismatic coordination of the Ce3+ ion. One macrocyclic ligand is additionally coordinated by a [Li(thf)]+ fragment. The coordination of the Li ion is square pyramidal.
    Notes: CeBr3 reagiert mit [(TMTAA)Li2] in THF zu dem paramagnetischen Doppeldeckerkomplex [Li(thf)][(TMTAA)2Ce], der mit 1 Mol THF pro Formeleinheit kristallisiert. Der Aufbau konnte durch eine Kristallstrukturanalyse aufgeklärt werden (Raumgruppe C2 (Nr. 5), Z = 6, a = 1741,8(2) pm, b = 1622,1(2) pm, c = 2540,4(3) pm, β = 104,72(1)°). Durch die sandwichartige Anordnung der TMTAA-Liganden erhält das Ce3+-Ion eine quadratisch-prismatische Koordination. An einen der makrozyklischen Liganden koordiniert zusätzlich ein [Li(thf)]+-Fragment. Das Li-Ion besitzt tetragonal-pyramidale Umgebung.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 81-85 
    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)°).
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 703-706 
    ISSN: 0044-2313
    Keywords: SmIII dimeric 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 Dilithiumbiphenyl with SmBr3. The Crystal Structure of [(C24H16)SmBr(thf)2]2 · [C24H14]In THF SmBr3 forms with [(biph)Li2] the dimeric complex [(quaph)SmBr(thf)2]2 · [C24H14]. The structure was characterized by X-ray single crystal structure analysis (space group P1 (No. 2), Z = 1, a = 943.3(6) pm, b = 1 350.3(1) pm, c = 1 599.9(9) pm, α = 64.99(5)°, β = 89.02(5)°, γ = 73.02(6)°). The Sm iones are bridged by two Br iones. Coordination by one quaph and THF ligands leads to distorded octahedra coordination of the Sm iones. Additionally crystallizes one molecule dibenzonaphthacene.
    Notes: SmBr3 reagiert mit [(biph)Li2] in THF zu dem zweikernigen Komplex [(quaph)SmBr(thf)2]2 · [C24H14]. Der Aufbau konnte durch eine Kristallstrukturanalyse geklärt werden (Raumgruppe P1 (Nr. 2), Z = 1, a = 943,3(6) pm, b = 1 350,3(1) pm, c = 1 599,9(9) pm, α = 64,99(5)°, β = 89,02(5)°, γ = 73,02(6)°). Die Sm-Ionen werden durch zwei Br-Ionen verbrückt. Durch zusätzliche Koordination eines quaph- und zweier THF-Liganden ist jedes Sm-Ion verzerrt oktaedrisch koordiniert. Zusätzlich kristallisiert ein Molekül Dibenzonaphthacen mit aus.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 814-818 
    ISSN: 0044-2313
    Keywords: GdIII and SmIII octahedra complexes ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Complexes of the Lanthanoides with Bidentate Ligands. The Crystal Structures of [(C17H17N2)GdBr2(thf)2] and [(C17H17N2)3Ln] (L = Sm, Gd)Reaction of [(AIP)Li] with GdBr3 leads to a new mononuclear complex [(AIP)GdBr2(thf)2] 1. In contrast to this with SmI2 the compound [(AIP)3Sm] 2 is build up. Such complexes are also formed with Gd(OR*)3 (R* = OtBu2C6H3) and [(AIP)Li] in a 1:3 ratio, [(AIP)3Gd] 3. The structures of 1-3 were characterized by X-ray single crystal structure analysis (1: space group Pna21 (No. 33), Z = 4, a = 1 972.7(9) pm, b = 984.7(5) pm, c = 1 425.0(8) pm, α = β = γ = 90°; 2 · 2 THF: space group C2/c (No. 15), Z = 8, a = 3 644.4(9) pm, b = 1 437.5(5) pm, c = 2 334.4(7) pm, β = 1 21.07(6)°; 3: space group P2(1)/c (No. 14), Z = 4, a = 1 872.9(1) pm, b = 1 064.6(1) pm, c = 2 282.4(2) pm, β = 103.75(8)°).
    Notes: GdBr3 reagiert mit [(AIP)Li] zu dem einkernigen Komplex [(AIP)GdBr2(thf)2] 1. Mit SmI2 bildet sich dagegen überraschenderweise die Komplexverbindung [(AIP)3Sm] 2. Komplexe dieser Art bilden sich auch bei der Umsetzung von Gd(OR*)3 (R* = OtBu2C6H3) mit [(AIP)Li] im Verhältnis 1:3, [(AIP)3Gd] 3. Der Aufbau von 1-3 konnte durch Kristallstrukturanalyse geklärt werden (1: Raumgruppe Pna21 (Nr. 33), Z = 4, a = 1 972,7(9) pm, b = 984,7(5) pm, c = 1 425,0(8) pm, α = β = γ = 90°; 2 · 2 THF: Raumgruppe C2/c (Nr. 15), Z = 8, a = 3 644,4(9) pm, b = 1 437,5(5) pm, c = 2 334,4(7) pm, β = 1 21,07(6)°; 3: Raumgruppe P2(1)/c (Nr. 14), Z = 4, a = 1 872,9(1) pm, b = 1 064,6(1) pm, c = 2 282,4(2) pm, β = 103,75(8)°).
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1913-1919 
    ISSN: 0044-2313
    Keywords: YIII ; SmIII ; GdIII ; benzyl ; complexes ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Benzyl Complexes of the Lanthanides. Synthesis and Crystal Structures of [(C5Me5)2Y(CH2C6H5)(thf)], [(C5Me5)2Sm(CH2C6H5)2K(thf)2]∞, and [(C5Me5)Gd(CH2C6H5)2(thf)]YBr3 reacts with potassium benzyl and [K(C5Me5)] in THF to give KBr and the monobenzyl compound [(C5Me5)2 · Y(CH2C6H5)(thf)] 1. The analogous reaction with SmBr3 in THF leads to the polymeric product [(C5Me5)2Sm(CH2C6H5)2 ∞ K(thf)2]∞ 2, with GdBr3 to [(C5Me5)Gd(CH2C6H5)2(thf)] 3.The structures of 1-3 were determined by X-ray single crystal structure analysis: 1:Space group P1, Z = 2, a = 851.2(4) pm, b = 952.7(4) pm, c = 1858.6(8) pm, α = 79.90(4)°, β = 77.35(4)°, γ = 73.30(3)°.2:Space group P1, Z = 2, a = 903.3(2) pm, b = 1375.9(3) pm, c = 1801.1(4) pm, α = 100.92(3)°, β = 100.77°, γ = 98.25(3)°.3:Space group P21/n, Z = 8, a = 1458.2(5) pm, b = 927.8(3) pm, c = 3792.9(15) pm, β = 96.83(3)°.
    Notes: YBr3 reagiert in Gegenwart von K(C5Me5) mit Kaliumbenzyl in THF unter Abspaltung von KBr zu der Monobenzylverbindung [(C5Me5)2Y(CH2C6H5)(thf)] 1. Die entsprechende Umsetzung mit SmBr3 führt in THF zu der polymeren Verbindung [(C5Me5)2Sm(CH2C6H5)2K(thf)2]∞ 2, mit GdBr3 zu [(C5Me5)Gd(CH2C6H5)2(thf)] 3. Die Strukturen von 1-3 wurden jeweils durch Anfertigen einer Einkristallstrukturanalyse geklärt: 1: Raumgruppe P1, Z = 2, a = 851,2(4) pm, b = 952,7(4) pm, c = 1858,6(8) pm, α = 79,90(4)°, β = 77,35(4)°, γ = 73,30(3)°.2: Raumgruppe P1, Z = 2, a = 903,3(2) pm, b = 1375,9(3) pm, c = 1801,1(4) pm, α = 100,92(3)°, β = 100,77°, γ = 98,25(3)°.3: Raumgruppe P21/n, Z = 8, a = 1458,2(5) pm, b = 927,8(3) pm, c = 3792,9(15) pm, β = 96,83(3)°.
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