Mercurimetrische Bestimmung von organisch gebundenem Chlor und Brom im Dezimilligrammbereich

Dirseherl, A.; Erne, F.

doi:10.1007/bf01217117

Cited by 19 publications

(7 citation statements)

References 15 publications

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“…FD mass spectra were taken on a Finnigan MAT 711 A instrument (8 kV, 60 °C), modified by AMD; FAB mass spectra were recorded on a Finnigan MAT TSQ 70 (10 kV, 50 °C). Elemental analyses were performed with a Carlo Erba 1106 analyzer; Cl, F, and S analyses were carried out according to Schöniger and determined as described by Dirscherl and Erne, Brunisholz and Michot, and Wagner . Ru was analyzed according to the literature …”

Section: Methodsmentioning

confidence: 99%

Behavior of (Ether−phosphine)ruthenium(II) Complexes [(η⁶-C₆Me₆)RuH(P⌒O)][BF₄] Containing Reactive Ru−O and Ru−H Bonds toward Various Small Molecules and Their Application in Ring-Opening Metathesis Polymerization

et al. 1998

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The ruthenium(II) complexes [(η6-C6Me6)RuH(P⌒O)][BF4] (5a − c; P⌒O = η2-(O,P)-chelated ether−phosphine; a, Ph2PCH2CH2OCH3; b, Ph2PCH2C4H7O2 (C4H7O2 = 1,3-dioxanyl); c, Ph2PCH2C3H5O2 (C3H5O2 = 1,3-dioxolanyl)), each having a Ru−O and Ru−H functionality, were obtained by hydride abstraction from (η6-C6Me6)RuH2(P∼O) (4a − c, P∼O = η1-(P)-coordinated ligand) with Ph3CBF4. A facile Ru−O bond cleavage occurs when 5a − c are reacted with a variety of small molecules. Carbon monoxide, acetonitrile, tert-butyl isocyanide, and ethene were readily added to 5a − c, leading to the corresponding adducts [(η6-C6Me6)RuH(P∼O)L][BF4] (6a − c, 7a − c, 8a − c, 10a − c; L = CO, CH3CN, t-BuNC, C2H4). π/σ rearrangements with incorporation of the Ru−H bonds in 10a − c were not observed. If 5a − c were treated with carbon disulfide, both functionalities were required. Rupture of the Ru−O contact resulted in a π-CS2-coordinated intermediate followed by an insertion of CS2 into the Ru−H bond to give the dithioformato complexes [(η6-C6Me6)RuH(P∼O)(S2CH)][BF4] (9a − c). All compounds were obtained in excellent yields under mild conditions. The structures of 5a, 7c, 8c, and 9a were determined by single-crystal X-ray diffraction methods. Ring-opening metathesis polymerization of norbornene was achieved using complexes 5a − c as the catalyst precursors.

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Section: Methodsmentioning

confidence: 99%

Behavior of (Ether−phosphine)ruthenium(II) Complexes [(η⁶-C₆Me₆)RuH(P⌒O)][BF₄] Containing Reactive Ru−O and Ru−H Bonds toward Various Small Molecules and Their Application in Ring-Opening Metathesis Polymerization

et al. 1998

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“…Elemental analyses were performed with a Carlo Erba 1106 analyzer and Perkin-Elmer Model 4000 atomic absorption spectrometer. Cl analyses were carried out according to the method of Schöniger and analyzed as described by Dirschel and Erne . Rh was determined on a Perkin-Elmer Model 4000 atomic absorption spectrometer.…”

Section: Methodsmentioning

confidence: 99%

Comparative Studies on Ether−Phosphine-Assisted Exchange Processes in the Rhodium(III) and Iridium(III) Complexes ClMH₂(P⌒O)(P∼O)

Lindner¹,

Gierling²,

Keppeler³

et al. 1997

Organometallics

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The rhodium and iridium complexes ClRhH2(P⌒O)(P∼O) (2a,b) and ClIrH2(P⌒O)(P∼O) (3a) (P⌒O = η2(P,O) coordination, P∼O = η1(P) coordination of Cy2PCH2CH2OCH3 (a) and Cy2PCH2C4H7O (b); C4H7O = tetrahydrofuranyl) were subjected to dynamic NMR studies. They exhibit a fast fluxional behavior both of the two ether oxygen donors and of the two cis hydrides at room temperature. The exchange of the hydrides is assisted by the fact that one of the ether moieties simulates an external solvent. The complexes 2a,b show the same behavior as is suggested for the coordinatively unsaturated species ClRhH2(PPh3)2, which is generally postulated to be an active intermediate in the catalytic hydrogenation of olefins. In the course of the formation of 3a from its ortho-metalated (4a; = η2(P,CH2) coordination of Cy2PCH2CH2OCH2) and dihydrogen, one C−H bond of the methoxy group and an additional Ir−H bond were formed. This was confirmed by the corresponding reaction of 4a with D2 to give the analogous dideuterium complex 3a‘. The opposite behavior was observed when 4a was treated with DCl: one C−D and one Ir−Cl bond were formed in the complex Cl2IrH(P⌒O)(P∼O) (5a; one Cy2PCH2CH2OCH2D ligand) while the hydride remained at the metal. The 103Rh chemical shift has been determined for compound 2b.

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“…FAB mass spectra were recorded on a Finnigan MAT TSQ 70 (10 kV, 50 °C) spectrometer. Elemental analyses were performed with a Carlo Erba 1106 analyzer; C1 and S analyses were carried out according to Schbniger [7] and analyzed as described by Dirschel and Erne [8] and Wagner [9]. Ru was determined according to the literature [10].…”

Section: Methodsmentioning

confidence: 99%

“…The unexpected formation of the acetylide complex Ru(CO)(P ~ O)2(r/2-S2CH)(C~CPh) (8) air-stable crystalline solid and is soluble in polar solvents like CH2C12 and CHC13. The FAB mass spectrum of 8 shows a parent peak which corresponds to the fragment [Ru(CO)(P ~ O)2(r/2-S2CH)(C~CPh)] +.…”

Section: Synthesis Of Complex Ru(co)(p ~ O)e(~l Z-szch)(c=-cph) (8)mentioning

confidence: 99%

Reactions of ether-phosphine ruthenium hydride complexes with carbon disulfide and phenylacetylene: crystal structures of Ru(CO) Cl(P ∼ O)3(η2-S2CH and Ru(CO) Cl(P ∼ O)2(η2-S2CH)

Lindner

Lin

Geprägs

et al. 1996

Journal of Organometallic Chemistry

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Mercurimetrische Bestimmung von organisch gebundenem Chlor und Brom im Dezimilligrammbereich

Cited by 19 publications

References 15 publications

Behavior of (Ether−phosphine)ruthenium(II) Complexes [(η⁶-C₆Me₆)RuH(P⌒O)][BF₄] Containing Reactive Ru−O and Ru−H Bonds toward Various Small Molecules and Their Application in Ring-Opening Metathesis Polymerization

Behavior of (Ether−phosphine)ruthenium(II) Complexes [(η⁶-C₆Me₆)RuH(P⌒O)][BF₄] Containing Reactive Ru−O and Ru−H Bonds toward Various Small Molecules and Their Application in Ring-Opening Metathesis Polymerization

Comparative Studies on Ether−Phosphine-Assisted Exchange Processes in the Rhodium(III) and Iridium(III) Complexes ClMH₂(P⌒O)(P∼O)

Reactions of ether-phosphine ruthenium hydride complexes with carbon disulfide and phenylacetylene: crystal structures of Ru(CO) Cl(P ∼ O)3(η2-S2CH and Ru(CO) Cl(P ∼ O)2(η2-S2CH)

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Mercurimetrische Bestimmung von organisch gebundenem Chlor und Brom im Dezimilligrammbereich

Cited by 19 publications

References 15 publications

Behavior of (Ether−phosphine)ruthenium(II) Complexes [(η6-C6Me6)RuH(P⌒O)][BF4] Containing Reactive Ru−O and Ru−H Bonds toward Various Small Molecules and Their Application in Ring-Opening Metathesis Polymerization

Behavior of (Ether−phosphine)ruthenium(II) Complexes [(η6-C6Me6)RuH(P⌒O)][BF4] Containing Reactive Ru−O and Ru−H Bonds toward Various Small Molecules and Their Application in Ring-Opening Metathesis Polymerization

Comparative Studies on Ether−Phosphine-Assisted Exchange Processes in the Rhodium(III) and Iridium(III) Complexes ClMH2(P⌒O)(P∼O)

Reactions of ether-phosphine ruthenium hydride complexes with carbon disulfide and phenylacetylene: crystal structures of Ru(CO) Cl(P ∼ O)3(η2-S2CH and Ru(CO) Cl(P ∼ O)2(η2-S2CH)

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Behavior of (Ether−phosphine)ruthenium(II) Complexes [(η⁶-C₆Me₆)RuH(P⌒O)][BF₄] Containing Reactive Ru−O and Ru−H Bonds toward Various Small Molecules and Their Application in Ring-Opening Metathesis Polymerization

Behavior of (Ether−phosphine)ruthenium(II) Complexes [(η⁶-C₆Me₆)RuH(P⌒O)][BF₄] Containing Reactive Ru−O and Ru−H Bonds toward Various Small Molecules and Their Application in Ring-Opening Metathesis Polymerization

Comparative Studies on Ether−Phosphine-Assisted Exchange Processes in the Rhodium(III) and Iridium(III) Complexes ClMH₂(P⌒O)(P∼O)