Chemie polyfunktioneller liganden

Ellermann, Jochen; Lietz, Martin

doi:10.1016/s0022-328x(00)81014-1

Cited by 10 publications

(7 citation statements)

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“…Chemicals of the best available commercial grade were used: n-butyllithium (1.6  solution in n-hexane, MerckSchuchardt), PbCl 2 (Aldrich), 207 PbCO 3 (Campro Scientific), InCl 3 (Aldrich). HN(PPh 2 ) 2 (5) was prepared according to literature procedures [6] [35] . Ϫ IR: Perkin Elmer 983.…”

Section: Methodsmentioning

confidence: 99%

“…The IR spectroscopic data of 3 are listed in the Experimental Section. The assignments of the PϪC 6 H 5 modes [6] are based on the Whiffen nomenclature [24] in the more currently used description of Maslowsky [25] . The mass spectrum (EI) of 3 does not show the molecular ion peak of 3 ϩ , but instead shows the [M Ϫ PPh] fragment along with various peaks due to PϪN and PϪPh fragments.…”

Section: The Binuclear Lead(1؉) Complexmentioning

confidence: 99%

“…Compound 5 was identified by its IR spectrum [6] . It was not possible to anneal NMR tubes and so the NMR spectra of 4 contain signals of the impurity 5.…”

Section: The Binuclear Lead(1؉) Complexmentioning

confidence: 99%

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Synthesis and X-Ray Structures of Novel Lead(1+) and Indium(3+) Phosphazenide Complexes; Detailed207Pb-NMR Spectra of the207Pb-Labelled Dimeric Lead(1+) Species

Winkler¹,

Bauer²,

Heinemann³

et al. 1998

Eur. J. Inorg. Chem.

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The reaction of PbCl2 with LiN(PPh2)2 (1) at −78°C affords the P−P coupled phosphazene Ph2P−N=PPh2−PPh2=N−PPh2 (2) as an oxidation product and, as a reduction equivalent, the novel lead(1+) complex [(Pb1+)2(μ‐Ph2P···N···PPh2−)2](Pb−Pb) (3). The crystal structure determination of the red compound 3 shows a Pb−Pb bond length of 304.1(1) pm. The 31P‐ and 207Pb‐NMR spectra of 3 are complicated due to the presence of a higher order spin system (AA′A′′A′′′X for the mono‐207Pb isotopomer, AA′A′′A′′′XX′ for the bis‐207Pb isotopomer). Simulations of the 31P and 207Pb spectra both on material with natural isotope abundance and on the 207Pb‐labelled compound (3*) reveal a large Pb,Pb coupling constant of 7708 Hz, indicative of a covalent Pb−Pb bond. − Though InCl3 is diagonally related to PbCl2, no significant redox process is observed in the reaction between InCl3 and 1. The yellow crystals of [In3+(Ph2P···N···PPh2−)3] (4) that are obtained were also investigated by X‐ray analysis. These show a propeller‐like configuration of the three four‐membered chelate rings with indium(3+) as the centre.

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Section: Methodsmentioning

confidence: 99%

Section: The Binuclear Lead(1؉) Complexmentioning

confidence: 99%

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Synthesis and X-Ray Structures of Novel Lead(1+) and Indium(3+) Phosphazenide Complexes; Detailed207Pb-NMR Spectra of the207Pb-Labelled Dimeric Lead(1+) Species

Winkler¹,

Bauer²,

Heinemann³

et al. 1998

Eur. J. Inorg. Chem.

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“…Nicht mehr so extrem hydrolyseemp®ndlich sind die (18-Krone-6)-Derivate 7±9. In deren Festko Èrper-IR-Spektren lassen sich die lagekonstanten Phenylschwingungsbanden der P(C 6 H 5 ) 2 -Gruppen [3] leicht zuordnen (s. (1) …”

Section: Ir-spektrenunclassified

Chemie polyfunktioneller Molekäle, 130. Mitt. [1]: Rubidium- und Cäsium-bis(diphenylphosphanyl)amid – Synthesen, (18-Krone-6)-Komplexe, Spaltprodukte, Kristallstrukturen und Festkörper-NMR-Spektren

Ellermann

Bauer

Schütz

et al. 1998

Monatshefte fuer Chemie

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The metalation of bis(diphenylphosphanyl)amine, HN(PPh 2 ) 2 (5), with RbOtBu in the presence of N,N,N H ,N HH ,N HH -pentamethyldiethylenetriamine (PMDTA (3)) in toluene surprisingly affords the nearly PMDTA free RbN(PPh 2 ) 2 (6a). Recrystallization of 6a from tetrahydrofuran (THF) yields RbN(PPh 2 ) 2 Á 0.5 THF (6b). Compounds 6a, b crystallize in thin needles; however, these are not suitable for X-ray structure analyses. The reactions of 5 with MOtBu (M Rb, Cs) in the presence of 18-crown-6 in toluene yield the monomeric, pale yellow rubidium and caesium complexes [Rb(18-crown-6)(N(PPh 2 ) 2 )] (7) and [Cs(18-crown-6)(N(PPh 2 ) 2 )] (8), respectively. Allowing to stand a solution of 8 in THF for three months at 20 C results in a cleavage product of 8. This is identi®ed as the dimeric yellow complex [(Cs(18-crown-6)) 2 ("-N=P(H)Ph 2 ) 2 ] Á THF (9). The source of the hydrogen atom in the bridging phosphorane iminate anion [ a a n n N=P(H)Ph 2 ] À is uncertain. Compounds 7±9 are structurally characterized by X-ray analyses. These reveal that [N(PPh 2 ) 2 ] À acts as P-ligating chelate in 7, whereas it coordinates the Cs as N-donor as well as 2 C-donor with one phenyl group in 8. No phosphorus coordination is observed in 8. The two caesium cations in 9 are two-fold N-bridged by [ a a n n N=P(H)Ph 2 ] À . The coordination sphere of each caesium atom is completed by a 18-crown-6 ligand. The solid state 13 C NMR spectrum of 8 reveals dynamic phenomena (rotation of the 18-crown-6 ligand). In the solid state 31 P spectrum of 8, 31 P, 31 P±J-coupling is observed between the chemically non-equivalent phosphorus sites (J 390 Hz).

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“…1 kann als 1.3-difunktioneller P-Ligand chelatisierend [4,5] und metallverbrük-kend [5][6][7] wirken. Weiterhin ist der Wasserstoff der NH-Gruppe zur Ausbildung von Wasserstoffbrückenbindungen befähigt [5,7] und durch Metalle [8,9], wie z.B. Lithium [1,7], ersetzbar.…”

Section: Introductionunclassified

Chemie polyfunktioneller Liganden, 57 [1] Über Iridium(I)- und Platin(II)-Komplexe des Bis(diphenylphosphino)amins und die oxidative Addition kleiner Moleküle an Di[bis(diphenylphosphino)amin-P.P']iricUum(I)-chlorid / Chemistry of Polyfunctional Ligands, 57[1] About Iridium(I) and Platinum(II) Complexes of Bis(diphenylphosphino)amine and the Oxidative Addition of Small Molecules to Di[bis(diphenylphosphino)amine]iridium(I)-chloride

Ellermann

Mader

1980

Zeitschrift Für Naturforschung B

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R2PNHPR2 (1) (R = C6H5) reacts with [(μ-Cl)Ir(C8H12)]2 in a molar ratio of 4:1, to give the square planar, ionic complex [Ir(R2PNHPR2)2]Cl (2a). By reaction of 2a with NaBR4, [Ir(R2PNHPR2)2]BR4 (2b) is obtained. Treatment of 2 a with CO gives [Ir(CO)(R2PNHPR2)2]Cl (3a). The complex 3a is also formed by the reaction of 1 with Ir(CO)(PR3)2Cl (R = C6H5) and Ir(CO)2(p-H2N-C6H4-CH3)Cl. 3a undergoes metathesis with NH4PF6 to yield [Ir(CO)(R2PNHPR2)2]PF6 (3b). The N-deuterated derivative [Ir(CO)(R2PNDPR2)2]Cl (4) is made by H/D exchange from 3a with CH3OD. Oxidative additions of O2 , CS2, I2 and (SCN)2 to 2a yield [Ir(O2)(R2PNHPR2)2]Cl (5), [Ir(μ2-CS2)(R2PNHPR2)2]Cl (6), [Ir(I)2(R2PNHPR2)2]Cl (7) and [Ir(SCN)2(R2PNHPR2)2]Cl (8). Additionally K2[PtCl4] and 1 reacts to [Pt(R2PNHPR2)2]Cl2 (9). The new compounds are characterised, as far as possible, by their IR, FIR, Raman and 31P NMR spectra.

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Chemie polyfunktioneller liganden

Cited by 10 publications

References 36 publications

Synthesis and X-Ray Structures of Novel Lead(1+) and Indium(3+) Phosphazenide Complexes; Detailed207Pb-NMR Spectra of the207Pb-Labelled Dimeric Lead(1+) Species

Synthesis and X-Ray Structures of Novel Lead(1+) and Indium(3+) Phosphazenide Complexes; Detailed207Pb-NMR Spectra of the207Pb-Labelled Dimeric Lead(1+) Species

Chemie polyfunktioneller Molekäle, 130. Mitt. [1]: Rubidium- und Cäsium-bis(diphenylphosphanyl)amid – Synthesen, (18-Krone-6)-Komplexe, Spaltprodukte, Kristallstrukturen und Festkörper-NMR-Spektren

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