Oxidation of metallic palladium by nitrosyl tetrafluoroborate

Schramm, Robert F.; Wayland, Bradford B.

doi:10.1039/c19680000898

Cited by 28 publications

(22 citation statements)

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“…Von den im Titel aufgefu È hrten komplexen Kationen sind bereits die Strukturen des Tetrakis(acetonitril)palladium(II)-Kations in Salzen mit den Anionen [BF 4 ] ± [19] und [CH 3 CN´SnCl 5 ] ± [20] und des Bis-(acetonitril)gold(I)-Kations im Salz mit dem [SbF 6 ] ± [8] aus Einkristall-Ro È ntgenstrukturbestimmungen bekannt. Vom Tetrakis(acetonitril)platin(II)-Kation scheint nur eine Strukturuntersuchung durch EXAFS-Experimente in CH 3 CN-Lo È sung zu existieren [21].…”

Section: Ro è Ntgenstrukturanalysenunclassified

“…Nach Abschmelzen der Zuleitungen befinden sich ca. 200 g gereinigtes HSO 3 Darstellung des Adduktes CH 3 CN´SbF 5 . In eine kleine, trockene Sublimationsapparatur werden 2 ml SbF 5 und 10 ml CH 3 CN einkondensiert.…”

Section: Ausgangsverbindungenunclassified

“…B. nach [2]: Zur na È heren Charakterisierung derartiger Komplexe wurden bereits in den 60er Jahren IR-spektroskopische Messungen durchgefu È hrt. In einer ersten systematischen Studie konnten Reedijk, Zuur und Groneveld [5] zeigen, daû in den Komplexen ± verglichen mit den Wellenzahlen im freien Liganden ± die Frequenzen der CN-, CC-Streck-und NCC-Deformationsschwingungen ansteigen und die der CH 3 -Deformations-und CH 3 [3], Pt [4], als Katalysatoren in der organischen Synthese, z. B. in der Oligomerisierung von Alkenen und Alkinen bei 20°C und Normaldruck und in Friedel-Krafts-Alkylierungen von Benzol, um nur wenige der zahlreichen Anwendungsmo È glichkeiten zu nennen [6,7].…”

Section: Introductionunclassified

“…CN (fl) und in komplex gebundenem CH3 CN, die einen Fehler von etwa ± 2 cm ±1 aufweisen, sind in Tabelle 1 und 2 aufgefu È hrt. Das von Byler und Shriver untersuchte Addukt ist durch schichtweises Ûbereinanderkondensieren von SbF 5 und CH 3 CN und anschlieûendes Tempern des Kondensats hergestellt worden[14,15].…”

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Synthesen und Schwingungsspektren der homoleptischen Acetonitrilkomplex-Kationen [Au(NCCH3)2]+, [Pd(NCCH3)4]2+, [Pt(NCCH3)4]2+ und des Adduktes CH3CN · SbF5. Kristallstrukturen der Salze [M(NCCH3)4][SbF6]2 · CH3CN, M = Pd, Pt

Ahsen

Bley

Proemmel

et al. 1998

Z. anorg. allg. Chem.

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Die Solvolyse der homoleptischen Metallcarbonyl‐Salze [M(CO)4][Sb2F11]2, M = Pd, Pt, in Acetonitril bei 50 °C führt einerseits zu einem vollständigen Ligandenaustausch für die Kationen und andererseits zu einer Umwandlung der di‐oktaedrischen Anionen [Sb2F11]– in [SbF6]– und das molekulare Addukt CH3CN · SbF5 gemäß der Gleichung [M(CO)4][Sb2F11]2 + 7 CH3CN → [M(NCCH3)4][SbF6]2 · CH3CN + 2 CH3CN · SbF5 + 4 CO M = Pd, Pt Die Monosolvate [M(NCCH3)4][SbF6]2 · CH3CN fallen als Einkristalle an und werden durch Röntgenbeugung strukturell charakerisiert. Beide Salze sind isostrukturell. Die Kationen sind quadratisch planar, während die N–C–C‐Gruppen geringfügig von der idealen Linearität abweichen. Die neuen Acetonitrilkomplexe sowie [Au(NCCH3)2][SbF6] und das Addukt CH3CN · SbF5 werden umfassend schwingungsspektroskopisch untersucht.

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Section: Ro è Ntgenstrukturanalysenunclassified

Section: Ausgangsverbindungenunclassified

Section: Introductionunclassified

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Synthesen und Schwingungsspektren der homoleptischen Acetonitrilkomplex-Kationen [Au(NCCH3)2]+, [Pd(NCCH3)4]2+, [Pt(NCCH3)4]2+ und des Adduktes CH3CN · SbF5. Kristallstrukturen der Salze [M(NCCH3)4][SbF6]2 · CH3CN, M = Pd, Pt

Ahsen

Bley

Proemmel

et al. 1998

Z. anorg. allg. Chem.

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“…Toluene was dried and distilled from sodium under a nitrogen atmosphere. [Pd(CH 3 CH 2 CN) 4 ][BF 4 ] 2 , 6, and [Pd(h 3 -C 3 H 5 ) (solv) 2 ][SbF 6 ], 7, were prepared according to procedures by Schramm [14] and Mathew [5c] respectively. Methylaluminoxane (MAO) was received from Aldrich as a 10 wt.-% solution in toluene and was dried (50 8C, 3 h, 0.1 mm Hg) before use.…”

Section: Methodsmentioning

confidence: 99%

Addition Polymers of Strained Cyclic Olefins – Transition Metal Catalysed Polymerisations of the Cyclobutene Derivative Bicyclo[3.2.0]hept‐6‐ene

Curran

Risse

Boggioni

et al. 2008

Macro Chemistry & Physics

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Bicyclo[3.2.0]hept‐6‐ene was converted into the corresponding addition polymer poly(6,7‐bicyclo[3.2.0]heptylene) with the aid of early and late transition metal based olefin polymerisation catalysts. Moderate to very good yields (42–99%) of polymer were obtained with [Pd(NCEt)4][BF4]2, [(η3‐allyl)Pd(solv)2][SbF6], [(2,9‐dimethyl‐1,10‐phenanthroline)Pd(CH3)(NC(CH2)6CH3)][SbF6], and Cp2ZrCl2/MAO, using monomer to transition metal ratios between 50/1 and 250/1. Reaction occurs at the olefin π‐bond, and the four‐membered ring of the monomer is retained during polymerisation which differs from ring‐opening olefin metathesis polymerisation in which the four‐membered ring is opened. The nearly exclusively saturated structure of the polymer was confirmed by 1H and 13C NMR spectroscopy. It is proposed that the polymers consist of repeating units that are predominantly cis‐exo‐enchained. GPC analysis of the soluble polymers prepared with [Pd(NCEt)4][BF4]2 showed that the molecular mass values $\overline M _{\rm n}$(GPC) were in the range of 3 700 to 22 600.magnified image

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Synthesis, Structure and Complexation Ability of Novel Metalloreceptors Containing Two Pincer Complexes of Palladium(II)

et al. 2004

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Metalloreceptors 1a and 1b were synthesized by palladation of 42-and 54-membered crown ethers that have two SCSpincer ligand moieties. The X-ray crystallographic analysis reveals that the metalloreceptor 1b has a folded structure in which the two pincer-Pd moieties are stacked in a parallel manner. The metalloreceptor 1b recognizes the aromatic biMetalloreceptors have recently attracted much attention in supramolecular chemistry because the physical and chemical properties of the metal center can be applied in guest binding, sensing, and regulation of molecular functions.[1] In particular, the coordination of various ligands to metals is very useful for the formation of a stable supramolecular system.[2Ϫ6] Combination of the coordinate bonding and other intermolecular interactions provides a strong and selective recognition.Complexes between Pd and pincer ligands are useful as they provide a nice coordination site for host-guest interaction. [7] For example, crown ethers containing a Pd center inside the ring and molecular recognition have been reported.[8Ϫ10] Cooperative binding of the Pd unit and the crown ether moiety to nucleobases such as cytosine and adenine was observed in this system. [11,12] However, a host molecule containing several pincer complexes as a binding site has not been synthesized although this type of host is very interesting as a multi-point receptor.Here we report the synthesis, structure and molecular recognition ability of large macrocyclic hosts 1, which contain two pincer complexes of Pd II . The metallohosts are expected to bind bidentate guests of different sizes in the cavity because the framework of these hosts is flexible so as to cause induced-fit recognition (Scheme 1).Metallohosts 1 containing the two Pd centers were prepared according to Scheme 2. Diols 2a [13] and 2b [14] were treated with p-toluenesulfonyl chloride to afford 3a and 3b in 80% and 63% yield, respectively. Reaction of dithiol 4 [15] with 3a, 3b in the presence of K 2 CO 3 afforded diols 5a, 5b, [a] [16] yielded metallohosts 1a, 1b. All spectroscopic data are consistent with the formula of 1 (see Exp. Sect.). Palladation of 7 caused broadening of the 1 H NMR signals, probably due to the enhanced rigidity of the structure, which restricts the free rotation of the methylene group. On metallation, downfield shifts of the signals for the SCH 2 CH 2 protons (e.g. δ ϭ 2.60 for 7b, δ ϭ 3.32 for 1b, Figure 1) and the benzyl protons is observed. This is elucidated by the decreased electron-density of these protons. ESI-MS for 1b gave signals at m/z ϭ 614. Ϫ anion during the ESI-MS measurements). In addition, the X-ray crystallographic analysis clarified the structure of 1b (Figure 2). The two complex moieties exhibit square-planar geometry at Pd, with three donor atoms provided by the rigid SCS chelate. The PdϪS distances are in

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Oxidation of metallic palladium by nitrosyl tetrafluoroborate

Cited by 28 publications

References 0 publications

Synthesen und Schwingungsspektren der homoleptischen Acetonitrilkomplex-Kationen [Au(NCCH3)2]+, [Pd(NCCH3)4]2+, [Pt(NCCH3)4]2+ und des Adduktes CH3CN · SbF5. Kristallstrukturen der Salze [M(NCCH3)4][SbF6]2 · CH3CN, M = Pd, Pt

Synthesen und Schwingungsspektren der homoleptischen Acetonitrilkomplex-Kationen [Au(NCCH3)2]+, [Pd(NCCH3)4]2+, [Pt(NCCH3)4]2+ und des Adduktes CH3CN · SbF5. Kristallstrukturen der Salze [M(NCCH3)4][SbF6]2 · CH3CN, M = Pd, Pt

Addition Polymers of Strained Cyclic Olefins – Transition Metal Catalysed Polymerisations of the Cyclobutene Derivative Bicyclo[3.2.0]hept‐6‐ene

Synthesis, Structure and Complexation Ability of Novel Metalloreceptors Containing Two Pincer Complexes of Palladium(II)

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