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  • 1
    ISSN: 0044-2313
    Keywords: Dicyclopentadienyl [bis(trimethylsilyl)phosphanido]titanium, [Cp2TiP(SiMe3)2] ; μ-chloro-μ-bis(trimethylsilyl)arsanido-bis(dicyclopentadienyl)titanium, [(Cp2Ti)2ClAs(SiMe3)2] ; trichloro-bis[tris(trimethylsilyl)phosphane]titanium, [TiCl3{P(SiMe3)3}2] ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of [CpTiCl]2 and TiCl4 with LiE(SiMe3)2 (E = P, As) and P(SiMe3)3. The Crystal Structures of [Cp2TiP(SiMe3)2], [(Cp2Ti)2ClAs(SiMe3)2], and [TiCl3 {P(SiMe3)3}2][Cp2TiCl]2 reacts with LiP(SiMe3)2 to form the mono nuclear complex [Cp2TiP(SiMe3)2] (3). 3 has been characterized by X-ray crystal structure analysis. 3 is paramagnetic and Ti is coordinated by two Cp ligands and a P(SiMe3)2 group. The geometry about the phosphorus atom is nearly trigonal planar. As a result of π-interactions one can find a short Ti—P bond length of about 246.7 pm. In contrast to the formation of 3, the reaction of [Cp2TiCl]2 with LiAs(SiMe3)2 yields the dinuclear Ti complex [(Cp2Ti)2ClAs(SiMe3)2] (4). TiCl4 and P(SiMe3)3 react to from the complex [TiCl3{P(SiMe3)3}2] (2). The Ti atom in 2 is coordinated to three Cl1- and two P(SiMe3)3 ligands.
    Notes: [Cp2TiCl]2 reagiert mit LiP(SiMe3)2 zu dem einkernigen Komplex [Cp2TiP(SiMe3)2] (3). Die Struktur des paramagnetischen 3 konnte mit Hilfe einer Kristallstrukturanalyse aufgeklärt werden. Danach wird das Titanatom von 2 Cp-Liganden und einer P(SiMe3)2-Gruppe koordiniert. Die an P gebundenen Atome liegen dabei in einer Ebene mit dem P-Atom. Als ein Ergebnis der π-Wechselwirkung zwischen Ti und P beobachtet man eine kurze Ti—P-Bindungslänge von 246,7 pm. Dagegen reagiert [Cp2TiCl]2 mit LiAs(SiMe3)2 zu dem zweikernigen Komplex [(Cp2Ti)2ClAs(SiMe3)2] (4). Setzt man TiCl4 mit P(SiMe3)3 um, erhält man weiße Kristalle der Zusammensetzung [TiCl3 {P(SiMe3)3}2] (2). In 2 ist Ti trigonal bipyramidal an die Cl1-- und P(SiMe3)3-Liganden gebunden.
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  • 2
    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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  • 3
    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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  • 4
    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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  • 5
    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.
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  • 6
    ISSN: 0044-2313
    Keywords: Chromium ; Palladium ; Copper Phosphaneimine Complexes ; Syntheses ; IR Spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Silylated Phosphaneimine Complexes of Chromium(II), Palladium(II), and Copper(II). The Crystal Structures of [CrCl2(Me3SiNPMe3)2], [PdCl2(Me3SiNPEt3)2], and [CuCl2(Me3SiNPMe3)]2The title compounds have been prepared by the reaction of the silylated phosphaneimines Me3SiNPR3 (R = CH3, C2H5) with CrCl2(THF)2, PdCl2 and CuCl2, respectively, in dichloromethane suspensions. All donor-acceptor complexes were characterized by IR spectroscopy and by crystal structure determinations.[CrCl2(Me3SiNPMe3)2]: Space group Pccn, Z = 4, structure determination with 2104 observed unique reflections, R = 0.045. Lattice dimensions at -70°C: a = 1326.3, b = 1562.5, c = 1171.5 pm. Within the monomeric molecular structure the chromium atom is planarly coordinated within the trans-configuration of the Cl atoms and the N atoms with distances of Cr—Cl = 235.94 pm and Cr—N = 211.7 pm.[PdCl2(Me3SiNPEt3)2]: Space group P21/n, Z = 2, structure determination with 2412 observed unique reflections, R = 0.031. Lattice dimensions at 20°C: a = 917.3, b = 1390.2, c = 1161.7 pm, β = 95.80°. Within the monomeric molecular structure the palladium atom is planarly coordinated within the trans-configuration of the Cl atoms and the N atoms with distances of Pd—Cl = 222.9 pm and Pd—N = 209.5 pm.[CuCl2(Me3SiNPMe3)2]: Space group Pbca, Z = 4, structure determination with 1861 observed unique reflections, R = 0.067. Lattice dimensions at -70°C: a = 1440.2, b = 1205.1, c = 1536.5 pm. The compound forms centrosymmetric dimeric molecules, in which the Cu atoms are linked via almost symmetrical chloro-bridges with Cu—Cl distances of 231.4 pm. The distance Cu—N is 196.7 pm.
    Notes: Die Titelverbindungen entstehen bei der Einwirkung der silylierten Phosphanimine Me3SiNPR3 (R = CH3, C2H5) auf CrCl2(THF)2, PdCl2 und CuCl2 in Dichlormethan-Suspension. Die drei Donor-Acceptor-Komplexe werden durch ihre IR-Spektren und durch Kristallstrukturanalysen charakterisiert.[CrCl2(Me3SiNPMe3)2]: Raumgruppe Pccn, Z = 4, Strukturlösung mit 2104 unabhängigen beobachteten Reflexen, R = 0,045. Gitterkonstanten bei -70°C: a = 1326,3; b = 1562,5; c = 1171,5 pm. In der monomeren Molekülstruktur ist das Chromatom planar in der trans-Konfiguration von den Cl-Atomen und den N-Atomen der Phosphanimin-Liganden koordiniert mit Abständen Cr—Cl = 235,94 pm und Cr—N = 211,7 pm.[PdCl2(Me3SiNPEt3)2]: Raumgruppe P21/n, Z = 2, Strukturlösung mit 2412 unabhängigen beobachteten Reflexen, R = 0,031. Gitterkonstanten bei 20°C: a = 917,3; b = 1390,2; c = 1161,7 pm, β = 95,80°. In der monomeren Molekülstruktur ist das Palladiumatom planar in der trans-Konfiguration von den Cl-Atomen und den N-Atomen der Phosphaniminliganden koordiniert mit Abständen Pd—Cl = 222,9 pm und Pd—N = 209,5 pm.[CuCl2(Me3SiNPMe3)]2: Raumgruppe Pbca, Z = 4, Strukturlösung mit 1861 unabhängigen beobachteten Reflexen, R = 0,067. Gitterkonstanten bei -70°C: a = 1440,2; b = 1205,1; c = 1536,5 pm. Die Verbindung bildet zentrosymmetrische dimere Moleküle, in denen die Cu-Atome über nahezu symmetrische Chlorobrücken mit Cu—Cl-Abständen von 231,4 pm verknüpft sind. Der Abstand Cu—N beträgt 196,7 pm.
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  • 7
    ISSN: 0044-2313
    Keywords: Yttrium(III) ; samarium(II) ; benzyl complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Lanthanide Halides with Alkalibenzyl Compounds. Synthesis and Crystal Structures of [(tmeda)(C6H5CH2)2Y(μ-Br)2Li(tmeda)], [(tmeda)2SmBr(μ-Br)2Li(tmeda)] and [(dme)2SmBr(μ-Br)]2Alkali-benzyl compounds react via a metathesis reaction with lanthanide halides to benzyl complexes of the rare earths. Reaction of [(C6H5CH2)Li(tmeda)] with YBr3 leads to the complex [(tmeda)Y(C6H5CH2)2 (μ-Br)2Li(tmeda)] 1, in which Yttrium and lithium are linked via two bromide bridges. However, the reaction of [(C6H5CH2)Li(tmeda)] with SmBr3 in toluene/tmeda leads under reduction of the Sm ion to the compound [(tmeda)2SmBr(μ-Br)2Li(tmeda)] 2. 2 reacts with DME to yield the dimeric compound [(dme)2SmBr(μ-Br)]2 3. The structures of 1-3 were determined by X-ray single crystal structure analysis:1:Space group P21/c, Z = 4, a = 829.5(6) pm, b = 1477.9(11) pm, c = 2575.0(10) pm, β = 92.03(6)°,2:Space group P21, Z = 2, a = 954,7(3) pm, b = 1338.5(6) pm, c = 1244.9(5) pm, β = 107.51(3)°,3:Space group P1, Z = 1, a = 797.2(7) pm, b = 818.3(7) pm, c = 1169.7(8) pm, α = 100.96(6)°, β = 92.03(6)°, γ = 91.75(7)°.
    Notes: Alkalibenzylverbindungen reagieren mit Lanthanoidhalogeniden unter Salzabspaltung zu Benzylkomplexen der Seltenen Erden. [(C6H5CH2)Li(tmeda)] bildet mit YBr3 den Komplex [(tmeda)(C6H5CH2)2Y(μ-Br)2Li(tmeda)] 1, in dem das Yttriumion mit Lithium über zwei Bromo-Brücken verknüpft ist. Bei der Reaktion von [(C6H5CH2)Li(tmeda)] mit SmBr3 in Toluol/TMEDA erfolgt hingegen unter Reduktion die Bildung von [(tmeda)2SmBr(μ-Br)2Li(tmeda)] 2. Diese Verbindung bildet mit DME den zweikernigen Komplex [(dme)2SmBr(μ-Br)]2 3. Die Strukturen von 1, 2 und 3 wurden durch Einkristallstrukturanalyse geklärt:1:Raumgruppe P21/c, Z = 4, a = 829,5(6) pm, b = 1477,9(11) pm, c = 2575,0(10) pm, β = 92,03(6)°,2:Raumgruppe P21, Z = 2, a = 954,7(3) pm, b = 1338,5(6) pm, c = 1244,9(5) pm, β = 107,51(3)°,3:Raumgruppe P1, Z = 1, a = 797,2(7) pm, b = 818,3(7) pm, c = 1169,7(8) pm, α = 100,96(6)°, β = 92,03(6)°, γ = 91,75(7)°.
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  • 8
    ISSN: 0044-2313
    Keywords: Samarium complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Reactivity of Samarium Complexes with Bis(diphenylchalcogenophosphoryl)amides. The Structures of [{η2-(Ph2PS)2N}2Sm(thf)2],[{η3-(Ph2PSe)2N}{η2-(Ph2PSe)2N}Sm(thf)2],[{η3-(Ph2PSe)2N}2Sm(SePh)(thf)], and [{η3-(Ph2PSe)2N}2Sm(SeMes)(thf)]The reaction of potassium-bis(diphenylchalcogenophosphoryl)amides with [SmI2(thf)5] affords complexes containing divalent samarium ions. Different structural types were characterised [{η2-(Ph2PS)2N}2Sm(thf)2] 1 and [{η3-(Ph2PSe)2N}{η2-(Ph2PSe) 2N}Sm(thf)2] 2 The ligands bind either bidentate through the two chalcogen atoms or tridentate through the chalcogen atoms and the nitrogen atom. On oxidation of 2 with diphenyldiselenide and dimesityldiselenide complexes [{η3-(Ph2PSe)2N}2Sm(SePh)(thf)] 3 or [{η3-(Ph2PSe)2N}2Sm(SeMes)(thf)] 4 are formed.(1: Space group Pbca (No. 61), Z = 4, a = 10.761(3) Å, b = 17.677(9) Å, c = 29.179(9) Å;2: Space group P1 (No. 2), Z = 2, a = 11.152(3) Å, b = 17.727(9) Å, c = 17.777(6) Å, α = 75.33(3)°, β = 77.74(3)°, γ = 72.21(3)°;3: Space group P21/c (No. 14), Z = 4, a = 13.399(2) Å, b = 45.868(6) Å, c = 11.9110(10) Å, β = 106.422(10)°;4: Space group P21/n (No. 14), Z = 4, a = 12.034(2) Å, b = 36.533(3) Å, c = 14.6617(10) Å, β = 96.889(12)°)
    Notes: Durch Umsetzungen von Kalium-Bis(diphenylchalkogenophosphoryl)amid mit [SmI2(thf)5] bilden sich Komplexe mit zweiwertigen Samariumionen. Es werden verschiedene Strukturtypen charakterisiert: [{η2-(Ph2PS)2N}2Sm(thf)2] 1 bzw. [{η3-(Ph2PSe)2N}{η2-(Ph2PSe) 2N}Sm(thf)2] 2. Der Ligand bindet entweder zweizähnig über die beiden Chalkogenatome oder dreizähnig über die Chalkogenatome und das Stickstoffatom. Wird 2 mit Diphenyldiselenid oder Dimesityldiselenid oxidiert, bilden sich die Komplexe [{η3-(Ph2PSe)2N}2Sm(SePh)(thf)] 3 bzw. [{η3-(Ph2PSe)2N}2Sm(SeMes)(thf)] 4.(1: Raumgruppe Pbca, (Nr.61), Z = 4, a = 10,761(3) Å, b = 17,677(9) Å, c = 29,179(9) Å;2: Raumgruppe P1 (Nr.2), Z = 2, a = 11,152(3) Å, b = 17,727(9) Å, c = 17,777(6) Å, α = 75,33(3)°, β = 77,74(3)°, γ = 72,21(3)°;3: Raumgruppe P21/c (Nr. 14), Z = 4, a = 13,399(2) Å, b = 45,868(6) Å, c = 11,9110(10) Å, β = 106,422(10)°;4: Raumgruppe P21/n (Nr. 14), Z = 4, a = 12,034(2) Å, b = 36,533(3) Å, c = 14,6617(10) Å, β = 96,889(12)°)
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  • 9
    ISSN: 0044-2313
    Keywords: GdIII ; SmIII ; binuclear complex ; thioureato-ligand ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thioureato Brigded Binuclear Complexes of the Lanthanides Synthesis and Crystal Structure of [{PhC(NPh)NC(S)NEt2}{Et2NC(S)NH}LnBr(thf)]2 (Ln = Gd, Sm)The reaction of potassium-N-(diethylaminothiocarbonyl)-N′-phenyl-benzamidinat with LnBr3 (Ln = Gd, Sm) leads to the formation of the binuclear complexes [{PhC(NPh)NC(S)NEt2}{Et2NC(S)N}LnBr(thf)]2} (Ln = Gd 1, Sm 2). The two bridging thiureatoligands are probably built during the reaction of potassium with the starting ligand. Coordination by one N-(diethylaminothiocarbonyl)-N′-phenylbenzamidinato-ligand, one Br-ion and one THF-ligand leads to square antiprismatic coordination of the lanthanoids. The structures of both compounds were characterized by X-ray analysis (1: P1 (Nr.2), Z = 1, a = 12,006(4) Å, b = 12,245(4) Å, c = 13,612(3) Å, α = 70,55(3)°, β = 68,21(3)°, γ = 81,31(3)° 2: P1 (Nr.2), Z = 1, a = 11,803(3) Å, b = 12,344(5) Å, c = 12,797(8) Å, α = 103,07(5)°, β = 101,76(3)°, γ = 114,13(3)°)
    Notes: Bei der Reaktion von Kalium-N-(diethylaminothiocarbonyl)-N′-phenyl-benzamidinat mit LnBr3 (Ln = Gd, Sm) bilden sich die zweikernigen Komplexe [{PhC(NPh)NC(S)NEt2}{Et2NC(S)N}LnBr(thf)]2} (Ln = Gd 1, Sm 2). Die Lanthanoidionen werden durch zwei Thioureatoeinheiten verbrückt, die sich vermutlich schon bei der Metallierung des Liganden bilden. Durch zusätzliche Koordination eines N-(Diethylaminothiocarbonyl)-N′-phenyl-benzamidinato-Liganden sowie eines THF-Moleküls und eines Brom-Atoms erhält jedes Lanthanoidion eine quadratisch antiprismatische Koordination.Der Aufbau dieser Verbindungen konnte durch Kristallstrukturuntersuchungen geklärt werden (1: P1 (Nr.2), Z = 1, a = 12,006(4) Å, b = 12,245(4) Å, c = 13,612(3) Å, α = 70,55(3)°, β = 68,21(3)°, γ = 81,31(3)° 2: P1 (Nr.2), Z = 1, a = 11,803(3) Å, b = 12,344(5) Å, c = 12,797(8) Å, α = 103,07(5)°, β = 101,76(3)°, γ = 114,13(3)°)
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  • 10
    ISSN: 0044-2313
    Keywords: Zirconium ; vanadium ; hexanuclear Zr—S and V—Se complexes ; preparation ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Clusters of Zr and V. The Crystal Structures of [Cp6Zr6S9] and [V6Se8O(PMe3)6]The hexanuclear complexes [Cp6Zr6S9] (1) and [V6Se8O(PMe3)6] (2) have been prepared by the reaction of [CpZrCl3] with S(SiMe3)2 and [CpVCl2(PMe3)2] with Se(SiMe3)2, respectively. The structure of 1 consists of discrete [Cp6Zr6S9] molecules with a Zr6 octahedron, coordinated by μ3-Se ligands. In the centre of the Zr6-octahedron is a further μ6-S atom. One can find the same cluster structure in 2, but the V6 octahedron is capped by μ3-Se ligands and the cluster centre is occupied by an oxygen atom.
    Notes: Bei der Reaktion von [CpZrCl3] mit S(SiMe3)2, bzw. von [CpVCl2(PMe3)2] mit Se(SiMe3)2 entstehen die sechskernigen Komplexe [Cp6Zr6S9] (1) bzw. [V6Se8O(PMe3)6] (2). Die Struktur von 1 besteht aus einem Zr6-Oktaeder, dessen Polyederflächen von μ3-S-Liganden besetzt sind, und die Cp-Liganden sind η5 an die Zr-Atome gebunden. Auch in 2 liegt ein Oktaeder vor, das aus 6 V-Atomen gebildet wird und von μ3-Se-Liganden koordiniert wird. 1 und 2 enthalten jeweils im Clusterzentrum ein zusätzliches S-bzw. O-Atom.
    Additional Material: 1 Ill.
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