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  • Articles: DFG German National Licenses  (17)
  • Inorganic Chemistry  (17)
  • 1
    Electronic Resource
    Electronic Resource
    Synthesis and Characterization of Substituted Benzyl Zinc Derivatives - Molecular Structures of (tmeda) Li-CH (GeMe3)Ph, (tmeda)Zn(CH2Ph)2, (tmeda)Zn[CH(SiMe3)Ph]2, and (tmeda)Zn[CH(SiMe3)Ph]N(H)Si(SiMe3)3Dedicated to Professor Manfred Weidenbruch on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1499-1505 
    Details
    ISSN: 0009-2940
    Keywords: Lithium ; Zine ; Dibenzylzinc ; Tmeda complexes ; Heteroleptic alkylzinc amide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of lithium phenyl(trimethylsilyl)methanide with phenyl(trimethylsilyl)methylzinc chloride-tmeda in the presence of tmeda yields the addition product, a bis(tmeda)-lithium dialkylchlorozincate. The elimination of lithium chloride leads to the formation of a tmeda adduct of bis[phenyl-(trimethylsilyl)methyl]zinc. The metathesis reaction of phenyl(trimethylsilyl)methylzinc chloride-tmeda with lithium tris(trimethylsilyl)silylamide allows the isolation of the corresponding heteroleptic tmeda complex of an alkylzinc amide. The metalation of phenyl(trimethylstannyl)methane with butyllithium yields the transmetalation product benzyllithium. From the metathesis reaction of this lithium base with anhydrous zinc(II) chloride in the presence of tmeda, the tmeda adduct of dibenzylzinc crystallizes. The molecular structures of (tmeda)Li—CH(GeMe3)Ph, (tmeda)Zn(CH2Ph)2, (tmeda)Zn[CH(SiMe3)Ph]2, and (tmeda)Zn[CH(SiMe3)-Ph[N(H)Si(SiMe3)3 are reported. Whereas lithium bonds in an η3-fashion, the zinc atom forms a σ(Zn—C) bond. The extremely wide Zn—N—Si angle in (tmeda)Zn[CH(SiMe3)-Ph[N(H)Si(SiMe3)3 of 157° is remarkable.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301024
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  • 2
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    Electronic Resource
    Synthesis and Dynamic Behavior of the Dimeric, Monocyclic Barium Bis[bis(isopropyldimethylsilyl)phosphanide] - Molecular Structures of P(SiMe2Ph)3, of Monomeric (thf)4Ba[P(SiMe2iPr)2]2 and of the Dimer {(thf)2Ba[P(SiMe2iPr]2]2}2 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1035-1040 
    Details
    ISSN: 0009-2940
    Keywords: Phosphanes ; Bis(silyl)phosphanes ; Tris(silyl)phosphanes ; Phosphanides ; Barium bis(phosphanide) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Barium bis[bis(trimethylsily)amide] metalates bis(isopropyldimethylsilyl)phosphane (1) to yield nearly quantitatively the corresponding barium bis[bis(isopropyldimethylsilyl)phosphanide] (3). This compound shows a temperature-dependent monomer-dimer equilibrium in toluene solution. Both the isomers were characterized by X-ray crystal structure analyses. The monomeric derivatives precipitate as a tetrakis(tetrahydrofuran) complex with a P-Ba-P bond angle of 139.9°. The barium atoms of the monocyclic, centrosymmetric dimer are pentacoordinated by two tetrahydrofuran molecules, one terminal and two bridging phosphanide ligands. The endo- and exocyclic Ba-P distances with values of 332 and 316 pm, respectively, lie within the characteristic range.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290910
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  • 3
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    Contributions to the Chemistry of Boron, 214. Synthesis and Reaction Chemistry of Aminophosphanylboranes (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 379-397 
    Details
    ISSN: 0009-2940
    Keywords: Boranes, amino-, phosphanyl- ; Diphosphadiboretanes ; Triphosphatriborinanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Aminochlorophosphanylboranes, (R2N)B(Cl)P(SiMe3)2 (1a  -  d) and (R2N)B(Cl)PH2 (2a  -  d), are obtained from elimination reactions between aminochloroboranes and LiP(SiMe3)2 and LiPH2, respectively. Selected reaction chemistry of (i1-Pr2N)B(Cl)P(SiMe3)2] (1a) with NH3, Me3SiN3, Cr(CO)5 · NMe3, and W(CO)5 · NMe3 is described. The azide (i1-Pr2N)B(N3)P(SiMe3)2 (12a) is stable at 25°C; however, thermolysis at 80°C provides a novel six-membered ring compound [(i1-Pr2N)BN(SiMe3)P(SiMe3)]2 (13a). The reaction of (Ph2N)B(Cl)P(SiMe3)2 (1b) with LiP(SiMe3)2 produces the only isolable bis(phosphanyl)borane (5b), while combination of (R2N)B(Cl)Ph2 with LiPH2 · DME yields new diphosphadiboretanes 6 {(R2N)BPH}2 (R2N=i1-Pr2N, Ph2N and tmp=2,2,6,6-tetramethylpiperidino) and triphosphatriborinanes 7 {(R2N)BPH}3 (R2N=(Me3Si)2N, Me2N and Et2N). Two salts, [(i1-Pr2N) DME]2 (8a) and [tmpLi · DME]2 (8c) (DME=ethylene glycol dimethyl ether) are also isolated. The results of molecular structure determinations for [(i1-Pr2N)Bn(SiMe3)P(SiMe3)]2 (13a), [tmpBPH]2 (4c), [tmpBPH]2 · Cr(CO)5 (7c), {[(Me3Si)2N]BPH}3 (4d), {[(Me3Si)2N]BPH}3 · Cr(CO)5 (7d), (Ph2N)B[P(SiMe3)2]2 (5b), and [(i1-Pr2N) · DME]2 (8a) are discussed.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260215
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  • 4
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    Synthese, Eigenschaften und Struktur von Amin-Addukten der Lithium-tris[bis(trimethylsilyl)methyl]zinkate (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 675-689 
    Details
    ISSN: 0044-2313
    Keywords: Lithium zincate ; tris[bis(trimethylsilyl)methyl]zincate ; x-ray structure ; NMR data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Properties, and Structure of the Amine Adducts of Lithium Tris[bis(trimethylsilyl)methyl]zincates.Bis[bis(trimethylsilyl)methyl]zinc and the aliphatic amine 1,3,5-trimethyl-1,3,5-triazinane (tmta) yield in n-pentane the 1:1 adduct, the tmta molecule bonds as an unidentate ligand to the zinc atom. Bis[bis(trimethylsilyl)methyl]zinc · tmta crystallizes in the triclinic space group P1 with {a = 897.7(3); b = 1 114.4(4); c = 1 627.6(6) pm; α = 90.52(1); β = 103.26(1); γ = 102.09(1)°; Z = 2}. The central C2ZnN moiety displays a nearly T-shaped configuration with a CZnC angle of 157° and Zn—C bond lengths of 199 pm. The Zn—N distances of 239 pm are remarkably long and resemble the loose coordination of this amine; a nearly complete dissociation of this complex is also observed in benzene. The addition of aliphatic amines such as tmta or tmeda to an equimolar etheral solution of lithium bis(trimethylsilyl)methanide and bis[bis(trimethylsilyl)methyl]zinc leads to the formation of the amine adducts of lithium tris[bis(trimethylsilyl)methyl]zincate. Lithium tris[bis(trimethylsilyl)methyl]zincate · tmeda · 2 Et2O crystallizes in the orthorhombic space group Pbca with {a = 1 920.2(4); b = 2 243.7(5); c = 2 390.9(5) pm; Z = 8}. In the solid state solvent separated ions are observed; the lithium cation is distorted tetrahedrally surrounded by the two nitrogen atoms of the tmeda ligand and the oxygen atoms of both the diethylether molecules. The zinc atom is trigonal planar coordinated; the long Zn—C bonds with a value of 209 pm can be attributed to the steric and electrostatic repulsion of the three carbanionic bis(trimethylsilyl)methyl substituents.
    Notes: Bis[bis(trimethylsilyl)methyl]zink reagiert in n-Pentan mit dem aliphatischen Amin 1,3,5-Trimethyl-1,3,5-triazinan (TMTA) unter Bildung des 1:1-Adduktes, wobei das TMTA-Molekül als einzähniger Ligand an das Zinkatom bindet. Das Bis[bis(trimethylsilyl)methyl]zink · TMTA kristallisiert in der triklinen Raumgruppe P1 mit {a = 897,7(3); b = 1 114,4(4); c = 1627,6(6) pm; α = 90,52(1); β = 103,26(1); γ = 102,09(1)°; Z = 2}. Das zentrale C2ZnN-Fragment weist mit einer nahezu T-förmigen Konfiguration einen CZnC-Winkel von 157° und Zn—C-Bindungslängen von 199 pm auf. Der Zn—N-Abstand von 239 pm ist außerordentlich lang und spricht für eine nur lockere Koordination des Amins, die durch eine weitgehende Dissoziation dieses Komplexes in Benzol bestätigt wird. Die Addition aliphatischer Amine wie TMEDA oder TMTA zu einer äquimolaren etherischen Lösung von Lithium-bis(trimethylsilyl)methanid und Bis[bis(trimethylsilyl)methyl]-zink führt zur Bildung der Amin-Addukte des Lithium-tris[bis(trimethylsilyl)methyl]zinkats. Das Lithium-tris-[bis(trimethylsilyl)methyl]zinkat · TMEDA · 2 Et2O kristallisiert in der orthorhombischen Raumgruppe Pbca mit {a = 1 920,2(4); b = 2 243,7(5); c = 2 390,9(5) pm; Z = 8}. Es liegen solvensgetrennte Ionen vor; das Lithiumkation ist verzerrt tetraedrisch von den Stickstoffatomen des TMEDA-Liganden und den Sauerstoffatomen der beiden Diethylether-Moleküle umgeben. Das Zinkatom ist trigonal planar koordiniert, die langen Zn—C-Bindungen von 209 pm erklären sich aus der sterischen und elektrostatischen Abstoßung der drei carbanionischen Bis(trimethylsilyl)methyl-Substituenten.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190409
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  • 5
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    Synthese und Molekülstruktur von Barium-bis[N,N′-bis(trimethylsilyl)benzamidinat] · DME · THF (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1455-1461 
    Details
    ISSN: 0044-2313
    Keywords: Barium-bis[N,N′-bis(trimethylsilyl)benzamidinate] · DME · THF ; Benzamidinate ; X-ray Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Molecular Structure of Barium Bis[N,N′-bis(trimethylsilyl)benzamidinate] ° DME ° THFBarium bis[N,N′-bis(trimethylsilyl)benzamidinate] · thf · dme crystallizes in the monoclinic space group P21/n with a = 1 122.0(2), b = 2 190.7(4), c = 1 840.2(3) pm, β = 98.04(1)° and Z = 4 containing a metal center in a distorted monocapped trigonal prismatic surrounding. The barium dibenzamidinate moiety is sent with an angle of 120°, although this leads to different Ba—N distances of 273 and 282 pm originating from the interligand repulsion of the trimethylsilyl groups and the dme substituent. The 1,3-diazaallyl fragment with C—N bond lengths of 132 pm shows a delocalisation of the anionic charge.
    Notes: Barium-bis[N,N′-bis(trimethylsilyl)-benzamidinat] · DME · THF kristallisiert in der monoklinen Raumgruppe P21/n mit a = 1 122,0(2), b = 2 190,7(4), c = 1 840,2(3) pm, β = 98,04(1)° und Z = 4 mit einem Metallzentrum in einer einfach überdachten, verzerrt prismatischen Umgebung. Die Barium-dibenzamidinat-Substruktur ist mit einem Winkel von 120° gewinkelt, die zwei jeweils verschiedenen Ba—N-Abstände von 273 und 282 pm rühren von der sterischen Hinderung zwischen den Trimethylsilyl-Gruppen und dem DME-Liganden her. Das 1,3-Diazaallyl-Fragment weist mit C—N-Bindungslängen von 132 pm eine Delokalisation der anionischen Ladung auf.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190822
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  • 6
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    [1,1,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5-diphosphet]trimethylaluminiuin und -indiumProfessor Walter Siebert zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 919-928 
    Details
    ISSN: 0044-2313
    Keywords: 1λ5, 3λ5-diphosphete ; aluminium ; indium complexes ; n.m.r ; mass ; ir spectra ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [1,l,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5-diphosphet]trimethylaluminiuin and -indium1,1,3,3-Tetrakis(dimethylamino)-1λ5, 3λ5-diphosphet, 1, reacts with A1(CH3)3 and In(CH3)3 to give the complexes [l,l,3,3-tetrakis(dimethylamino)-1λ5, 3λ5-diphosphete]-trimethylaluminium, 2, and [1,1,3,3-Tetrakis(dimethylamino)-l,1λ5, 3λ55-diphosphete]-trimethylindium, 3, as crystalline products, respectively. Properties, n.m.r., mass and i.r. spectra are reported and interpreted. Compounds 2 and 3 are further characterized by X-ray structural analyses; the bonding situation in both complexes is discussed in detail
    Notes: 1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet, 1, reagiert mit Al(CH3)3 bzw. In(CH3)3 zu den Komplexen [1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet]trimethylaluminium, 2, bzw. [1,1,3,3-Tetrakis(dimethylamino)-1λ5,3λ5-diphosphet]trimethylindium, 3, die jeweils als kristalline Produkte erhalten werden. Die Eigenschaften, NMR-, Massen- und IR-Spektren werden mitgeteilt und interpretiert. 2 und 3 sind zusätzlich durch Kristallstrukturanalysen charakterisiert; die Bindungsverhältnisse in beiden Komplexen wurden eingehend diskutiert.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.199762301145
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  • 7
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    Synthese von Magnesium-bis[N,N′-bis(trimethylsilyl)benzamidinat] als Bis(THF)- und Benzonitril-Addukt (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 27-34 
    Details
    ISSN: 0044-2313
    Keywords: Magnesium, N,N′-Bis(trimethylsi yl)benzamidinate ; synthesis ; spectroscopic data ; structure of magnesium bis[N,N′-bis(trimethylsilyl)benzamidinate] ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis of Magnesium Bis[N,N′ -bis(trimethylsilyl)benzamidinate] as both Bis(THF) and Benzonitrile AdductMagnesium bis[bis(trimethylsilyl)amide] 1, reacts with benzonitrile in toluene at room temperature to yield magnesium bis[N,N′-bis(trimethylsilyl)benzamidinate]-benzonitrile(1/1) 2. Addition of THF leads to a quantitative substitution of the benzonitrile ligand by two THF molecules. The performance of the addition reaction in THF yields magnesium bis[N,N′-bis(trimethylsilyl)benzamidinate] · THF(1/2) 3. The upper benzonitrile complex 2, crystallizes in the orthorhombic space group Pbcn with {a = 1383.2(2); b = 2589.1(4); c = 1133.7(1) pm; Z = 4}. The magnesium atom is coordinated distorted trigonal-bipyramidal, where the benzonitrile ligand lies within the equatorial plane. The axial bound nitrogen atom of the benzamidinate substitution shows with a value of 213 pm a slightly longer bond distance to the metal center than the one in the equatorial plane (210 pm). The steric strain within the benzamidinate ligand leads to an elongation of the silicon atoms out of the 1,3-diazaallylic moiety under an enlargement of the C—N—Si angle to 131°.
    Notes: Magnesium-bis[bis(trimethylsilyl)amid] 1, reagiert mit Benzonitril in Toluol bei Zimmertemperatur zu Magnesium-bis[N,N′-bis(trimethylsilyl)benzamidinat]-Benzonitril(1/1) 2. Der Benzonitriligand läßt sich durch Zugabe von THF quantitativ durch zwei Ethermoleküle ersetzen. Auch die Durchführung der Additionsreaktion in THF führt zum Magnesium-bis [N,N′ -bis(trimethylsilyl)benzaminidat]-THF(1/2) 3. Der erstgenannte Benzonitril-Komplex 2, kristallisiert in der orthorhombischen Raumgruppe Pbcn mit {a = 1383,2(2); b = 2589,1(4); c = 1133,7(1) pm; Z = 4}. Das Magnesiumatom weist verzerrt trigonal-bi-pyramidale Umgebung auf, wobei sich der Benzonitrilligand in der äquatorialen Ebene anordnet. Das in der axialen Position befindliche Stickstoffatom des Benzamidinat-Substituenten weist mit 213 pm einen um etwa 3 pm größeren Abstand zum Metallzentrum auf als dasjenige in der äquatorialen Ebene. Die sterischen Spannungen innerhalb des Benzamidinat-Liganden führen zur Auslenkung der Siliciumatome aus der 1,3-Diazaallylebene unter gleichzeitiger C—N—Si-Winkelaufweitung auf 131°.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926150906
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  • 8
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    Strontium- und Barium-bis[N,N′ -bis(trimethylsilyl)benzamidinate] aus der Additionsreaktion der Erdalkalimetall-bis[bis(trimethylsilyl)amide] mit Benzonitril (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 121-130 
    Details
    ISSN: 0044-2313
    Keywords: Benzamidinates ; Strontium-bis[N,N′-bis(trimethylsilyl)benzamidinate] ; Barium-bis[N,N′-bis(trimethylsilyl)benzamidinate] ; X-ray Structures ; Spectroscopic Data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strontium and Barium Bis[N,N′-bis(trimethylsilyl)benzamidinates] from the Addition Reaction of the Alkaline Earth Metal Bis[bis(trimethylsilyl)amides] and BenzonitrileThe reaction of strontium bis[bis trimethylsilyl)amide] with benzonitrile yields strontium bis[N,N′- bis(trimethylsilyl)benzamidinate] · 2THF, which crystallizes in the orthorhombic space group Pbcn (a = 1845.4(3); b = 131 1,3(2); c = 1838,(3) pm; Z = 4). During the similar reaction of barium bis[bis(trimethylsilyl)amide] with benzonitrile the benzonitrile adduct barium bis[N,N′-bis(trimethylsilyl)benzamidinate] · 2 THF · benzonitrile is formed. After the addition of diphenylacetylene to the strontium di(benzamidinate) in diglyme a clathrate of the composition strontium bis[N,N′-bis(trimethylsilyl)benzamidinate] · diglyme · diphenylacetylene could be isolated; the spectroscopic data as well as the X-ray structure (monoclinic, C2/c, a = 1492.2(2); b = 1539.1(2); c = 2337.8(3)pm; Z = 4) confirm the isolated appearance of the acetylene molecule without interaction to the metal center in solution and in the solid state, respectively.
    Notes: Bei der Umsetzung des Strontiumbis[bis(trimethylsilyl)amids] mit Benzonitril in THF bildet sich Stronitium-bis[N,N′-bis(trimethylsilyl)benzamidinat] · 2THF, das in der orthorhombischen Raumgruppe Pbcn mit {a = 1 845,4(3); b = 1311,4(2); c = 1838,8(3) pm, Z = 4} kristallisiert. Die entsprechende Reaktion des Barium-bis[bis(trimethylsilyl)amids] mit Benzonitril ergibt das Benzonitril-Addukt Barium bis[N,N′ -bis(trimethylsilyl)benzamidinat] · 2 THF · Benzonitril. Nach der versuchsweisen Umsetzung des Strontium-di(benzamidinats) mit Diphenylacetylen in Diglyme läßt sich ein Clathrat der Zusammensetzung Strontiumbis[N,N′-bis(trimethylsilyl)benzamidinat] · Diglyme · Diphenylacetylen erhalten, dessen spektroskopische und strukturanalytische Untersuchungen (monoklin, C2/c, a = 1492,2(2); b = 1539,1(2); c = 2337,8(3) pm; β = 100,74(1)°; Z = 4) das Vorliegen eines unkomplexierten Diphenylacetylen-Moleküls sowohl in Lösung als auch im Festkörper bestätigen.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926180121
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  • 9
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    Tris[bis(trimethysilyl)amido]zinkate von Lithium und Calcium (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 618 (1992), S. 131-138 
    Details
    ISSN: 0044-2313
    Keywords: Tris[bis(trimethylsilyl)amido]zincate ; Zincate ; Lithium-zincate ; Calcium-bis(zincate) ; Spectroscopic Data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tris[bis(trimethylsilyl)amido]zincates of Lithium and CalciumCalcium-bis[bis(trimethylsilyl)amide] and Bis[bis(trimethylsilyl)amido]zinc yield in 1,2-dimethoxyethane quantitatively Calcium-bis{tris[bis(trimethylsilyl)- amido]zincate} · 3DME. When THF is chosen as a solvent, the two reactants and the zincate form a temperature-independent equilibrium, whereas in benzene no reaction occurs. The tris[bis(trimethylsilyl)amido]zincate anion displays characteristic 13C{1H) and 29Si{1H] chemical shifts of 7 and -8 ppm, respectively; the nature of the solvent, the cation and the complexating ligands don't influence the IR nor NMR data of the zincate anion and thus verify that [Ca(DME)3]2+ and {Zn[N(SiMe3 2]3}- appear as solvent separated ions, which is also confirmed by their insolubility in hydrocarbons.
    Notes: Calcium-bis[bis(trimethylsilyl)amid] und Bis[bis(trimethylsilyl)amido]zink reagieren in 1,2-Dimethoxyethan quantitativ zum Calcium-bis[tris[bis(trimethylsilyl)amido]zinkat} · 3DME. In THF bilden diese Reaktanden und das aus ihnen gebildete Zinkat ein Temperatur-unabhängiges Gleichgewicht, wohingegen in Benzol keine Reaktion beobachtet wird. Das Tris[bis(trimethylsilyl)amido]zinkat-Anion weist charakteristische chemische Verschiebungen im 13C{1H}- bzw. 29Si{1H}- NMR-Spektrum von 7 und - 8 ppm auf; die Art des Lösungsmittels, das Kation und die Komplexliganden beeinflussen die IR- und NMR-Parameter des Zinkatanions kaum und legen das Vorliegen solvensgetrennter Ionen [Ca(DME)3]2+ und {Zn[N(SiMe3)2]3}- nahe, was auch durch die Unlöslichkeit dieser Zinkate in Kohlenwasserstoffen bestätigt wird.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19926180122
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  • 10
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    Tris(trimethylsilyl)silylamin und seine lithiierten und silylierten Derivate  -  Kristallstruktur des dimeren Lithium-trimethylsilyl-[tris(trimethylsilyl)silyl]amids (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1053-1063 
    Details
    ISSN: 0044-2313
    Keywords: Tris(trimethylsilyl)silyltriflate ; Tris(trimethylsilyl)silylamine ; Lithium Amide ; X-Ray Structure ; Spectroscopic Data ; Agostic Interactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tris(trimethylsilyl)silylamine and the lithiated and silylated Derivatives  -  X-Ray Structure of the dimeric Lithium Trimethylsilyl-[tris(trimethylsilyl)silyl]amideThe ammonolysis of the chlor, brom or trifluormethanesulfonyl tris(trimethylsilyl)silane yields the colorless tris(trimethylsilyl)silylamine, destillable at 51°C and 0.02 Torr. The subsequent lithiation, reaction with chlor trimethylsilane and repeated lithiation lead to the formation of lithium tris(trimethylsilyl)silylamide, trimethylsilyl-[tris(trimethylsilyl)silyl]amine and finally lithium trimethylsilyl-[tris(trimethylsilyl)silyl]amide, which crystallizes in the monoclinic space group P21/n with a = 1 386.7(2); b = 2 040.2(3); c = 1 609.6(2) pm; β = 96.95(1)° and Z = 4 dimeric molecules. The cyclic Li2N2 moiety with Li—N bond distances displays a short transannular Li … Li contact of 229 pm. The dimeric molecule shows nearly C2-symmetry, so that one lithium atom forms agostic bonds to both the trimethylsilyl groups, the other one to the tris(trimethylsilyl)silyl substituents. However, the 7Li{1H}-NMR spectrum displays a high field shifted singlet at  - 1.71 ppm. The lithiation of trimethylsilyl-[tris(trimethylsilyl)silyl]amine leads to a high field shift of the 29Si{1H} resonance of about 12 ppm for the Me3SiN group, whereas the parameters of the tris(trimethylsilyl)silyl ligand remain nearly unaffected.
    Notes: Die Ammonolyse von Chlor-, Brom- oder Trifluormethansulfonyl-tris(trimethylsilyl)silan ergibt das bei 51°C/0,02 Torr zu destillierende, farblose Tris(trimethylsilyl)silylamin. Durch Lithiierung erhält man das in Benzol dimer vorliegende Lithium-tris(trimethylsilyl)silylamid; die anschließende Umsetzung mit Chlortrimethylsilan und abermalige Lithiierung führen zu dem in Benzol ebenfalls dimer auftretenden Lithiumtrimethylsilyl-[tris(trimethylsilyl)silyl]amid, das in der monoklinen Raumgruppe P21/n mit a = 1 386,7(2); b = 2 040,2(3); c = 1 609,6(2) pm; β = 96,95(1)° und Z = 4 Dimeren kristallisiert. Das zentrale Strukturelement bildet der Li2N2-Cyclus mit Li—N-Abständen um 202 pm und einem kurzen Li … Li-Kontakt von 229 pm. Das dimere Molekül weist nahezu C2-Symmetrie auf, so daß das eine Lithiumatom agostische Bindungen zu den zwei Trimethylsilyl-Gruppen, das andere hingegen zu den Tris(trimethylsilyl)silyl-Substituenten aufweist, allerdings läßt sich in benzolischer Lösung 7Li{1H}-NMR-spektroskopisch nur ein Hochfeld-verschobenes Singulett bei  -  1,71 ppm beobachten. Im 29Si{1H}-NMR-Spektrum läßt sich durch die Lithiierung des Trimethylsilyl-[tris(trimethylsilyl)silyl]amins eine Hochfeldverschiebung um 12 ppm für den Me3SiN-Rest registrieren, während die NMR-Parameter des Tris(trimethylsilyl)silyl-Liganden eine nur geringe Verschiebung erfahren.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190616
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