Sur le dosage volumétrique du fluor

Brunisholz, G.; Michod, J

doi:10.1002/hlca.19540370223

Cited by 32 publications

(2 citation statements)

References 7 publications

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“…The assignment of the signals has been supported by DEPT-135, homonuclear, and heteronuclear correlation spectra. Elemental analyses were performed with a Carlo Erba 1106 analyzer; F and S analyses were carried out according to Schöniger and determined as described by Brunisholz and Michod and Wagner, respectively. Rhenium, ruthenium and osmium were determined with a Varian AA20.…”

Section: Methodsmentioning

confidence: 99%

Synthesis, Structure, and Electrochemistry of Osmametallocenophanes with Different Ring Size^,¹

et al. 1999

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The reaction of the bis(triflates) [η5-C5H4(CH2) n OTf]2M (n = 3, M = Fe (4a), Ru (5a); n = 4, M = Fe (4b), Ru (5b); n = 6, M = Fe (4c), Ru (5c)), which are obtained from the bis(alcohols) [η5-C5H4(CH2) n OH]2M (2a − c, 3a − c) and (CF3SO2)2O in the presence of pyridine, with Na2[Os(CO)4] in dimethyl ether results in the formation of the novel osmametallocenophanes [η5-C5H4(CH2) n Os(CO)4(CH2) n C5H4-η5]M (6a − c, 7a − c). The structures of 6b (n = 4, M = Fe) and 7c (n = 6, M = Ru) were investigated by X-ray structural analyses. In a similar way the bis(rhenium) complexes [η5-C5H4(CH2) n Re(CO)5]2M (8a − c, 9a − c) were made accessible from the bis(triflates) 4a − c and 5a − c and Na[Re(CO)5] in THF. The dependence of the redox behavior of the metallocene unit in the osmametallocenophanes 6a − c and 7b,c on the metal−metal distance was examined by means of cyclic voltammetry. The obtained results were compared with those of the bis(alcohols) 2a − c and 3a − c and the bis(rhenium) complexes 8a − c and 9a − c. The ferrocenes are characterized by a reversible one-electron oxidation, whereas the ruthenocenes feature an irreversible two-electron process accompanied by a chemical reaction. A consistent through-space effect of the spacer-bound substituents on the redox potential is observed in the case of the ferrocenes.

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Section: Methodsmentioning

confidence: 99%

Synthesis, Structure, and Electrochemistry of Osmametallocenophanes with Different Ring Size^,¹

et al. 1999

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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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Cage-Structured Triplatinacyclophanes

Lindner¹,

Hermann

Baum

et al. 1999

Eur. J. Inorg. Chem.

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The synthesis of the tris(triflate) 4 (Scheme 1) has been achieved by means of a straightforward three‐step reaction sequence. After initial lithiation of mesitylene, treatment of the obtained trilithium compound C6H3(CH2Li)3 (2) with oxirane results in the formation of 1,3,5‐tris(3‐hydroxypropyl)benzene (3), which is then transformed to 4 by reaction with (CF3SO2)2O in the presence of pyridine. Whereas 4 reacts with Na2[Os(CO)4] in a somewhat complicated manner, similar reactions with Na[Re(CO)5] and LiPPh2 give the hydrocarbon‐bridged tris(rhenium) complex C6H3[(CH2)3Re(CO)5]3 (5) and the tris(phosphane) C6H3[(CH2)3PPh2]3 (6), respectively. Employing the high‐dilution method, from 6 and Cl2Pt(NCPh)2 the nanoscaled tri‐ and hexaplatinacyclophanes 7 and 9 are available. Owing to the optimal geometry and flexibility of the cage in 7, 1,2‐dichloroethane can be reversibly encapsulated. The molecular structure of 7 · 7 1,2‐Cl2C2H4 was determined by an X‐ray structure analysis. The utility of the reactive metal centers in 7 has been demonstrated by replacing the chloro ligands by acetonitrile to give the cationic platinacyclophane 8, in which, according to NMR studies, the cage‐like structure is preserved.

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Sur le dosage volumétrique du fluor

Cited by 32 publications

References 7 publications

Synthesis, Structure, and Electrochemistry of Osmametallocenophanes with Different Ring Size^,¹

Synthesis, Structure, and Electrochemistry of Osmametallocenophanes with Different Ring Size^,¹

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

Cage-Structured Triplatinacyclophanes

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Sur le dosage volumétrique du fluor

Cited by 32 publications

References 7 publications

Synthesis, Structure, and Electrochemistry of Osmametallocenophanes with Different Ring Size,1

Synthesis, Structure, and Electrochemistry of Osmametallocenophanes with Different Ring Size,1

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

Cage-Structured Triplatinacyclophanes

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Product

Resources

About

Synthesis, Structure, and Electrochemistry of Osmametallocenophanes with Different Ring Size^,¹

Synthesis, Structure, and Electrochemistry of Osmametallocenophanes with Different Ring Size^,¹

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