Nitrogen-15 nuclear magnetic resonance spectroscopy of hydrazido(2–)-, imido-, and nitrido-complexes of molybdenum and tungsten

Donovan-Mtunzi, Susan; Richards, Raymond L.; Mason, Joan

doi:10.1039/dt9840001329

Cited by 38 publications

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“…A similar structure was proposed for a complex of nickel and P(C 6 H 11 ) 3 with bridging dinitrogen [9]. Moreover, NAN stretching frequencies in complexes with other metals also containing bridging dinitrogen [10,11] , the i.r. spectrum also shows a band of medium intensity at 1750 cm )1 assigned to the CAC stretching frequency of the bridging ethynediyl group.…”

Section: Resultssupporting

confidence: 69%

Compounds of triphenylstibine and platinum: synthesis, properties and reactivity

Barbieri

Bellato

Massabni

2005

Transition Met Chem

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The reactivity of [Pt(SbPh 3 ) 3 ], a compound of zerovalent platinum, exceptionally stable in air, is described. The compounds [{Pt(SbPh 3 ) 3 } 2 N 2 ], containing bridging dinitrogen, [{Pt(SbPh 3 ) 3 } 2 C 2 ], with an ethynediyl group also bridging, and [Pt(CO) 2 (SbPh 3 ) 2 ], were all obtained under ordinary pressure of nitrogen, acetylene or carbon monoxide, respectively, and are also described. Among the products of the reactions, the dimer [PtBr 3 (SbPh 3 ) 2 ] 2 and the mixed complexes [PtL 2 (SbPh 3 ) 2 ] (L = PPh 3 , AsPh 3 ) were also obtained. Some of these complexes are luminescent when excited by u.v. radiation.

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Section: Resultssupporting

confidence: 69%

Compounds of triphenylstibine and platinum: synthesis, properties and reactivity

Barbieri

Bellato

Massabni

2005

Transition Met Chem

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“…When a sample of 2 in [D 8 ]toluene was cooled and sealed under an atmosphere of 15 N 2 , three resonances were observed in the 15 N NMR spectrum at low temperature, consistent with both terminal binding (δ ϭ Ϫ47.9 and Ϫ112.4) and a bridged structure (δ ϭ Ϫ133). [13,14] The 31 P{ 1 H} resonances associated with these structures also exhibited coupling to 15 N.Concentration and cooling of a diethyl ether solution of 2 under argon afforded large purple-black crystals suitable for an X-ray diffraction study. The solid-state structure of 2 is shown in Figure 1.…”

mentioning

confidence: 99%

Synthesis and Chemistry of the 16-Electron Osmium Complex [OsBr(η5-C5Me5)(PiPr3)]

Glaser

Tilley

2001

Eur. J. Inorg. Chem.

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The isolable 16-electron half-sandwich Os complex [OsBr(η 5 -C 5 Me 5 )(PiPr 3 )] has been synthesized and structurally characterized. This unsaturated complex binds N 2 reversibly at lowThe stable 16-electron complexes [RuClCp*(PR 3 )] (Cp* ϭ η 5 -C 5 Me 5 ; R ϭ iPr, Cy) were reported in 1988. [1] These complexes, prepared by addition of the appropriate phosphane in one step from the tetrameric ruthenium species [RuClCp*] 4 , [2] have proven to be valuable starting materials for the synthesis of various silyl, [3] silene, [4] and metallacyclic [5] complexes. Analogous 16-electron complexes of osmium are also expected to be useful synthons, but they have yet to be reported. The synthesis of coordinatively unsaturated [OsXCp*(PR 3 )] species would seem to require a method other than that used to prepare the related ruthenium complexes, as the osmium analog of [RuClCp*] 4 is not known. However, Esteruelas and co-workers have recently reported [6] the preparation of an 18-electron complex, [OsClCp(PiPr 3 ) 2 ], which dissociates a phosphane ligand in solution to form an unsaturated species that activates EϪH bonds (E ϭ C, Si, Ge, Sn). [7,8] Addition of two equiv. of triisopropylphosphane to a stirred CH 2 Cl 2 solution of [Os 2 Br 4 Cp* 2 ] [9] effected a rapid color change from dark brown to black-cherry red. Removal of all volatile components of the mixture, washing with ether, and drying under vacuum afforded a pale pink-red solid which was soluble in toluene and dichloromethane. Three broad, featureless resonances spread over a range of greater than 30 ppm in the 1 H NMR spectrum (CD 2 Cl 2 , room temperature) were consistent with a paramagnetic 17-electron complex formulated as [OsBr 2 Cp*(PiPr 3 )] (1); however, a CH 2 Cl 2 solution of 1 gave no detectable EPR signal at room temperature, and only below 100 K was an extremely broad signal (with no detectable hyperfine coupling) observed. A Signer molecular weight determination [10,11] (room temperature, CH 2 Cl 2 solution) confirmed the monomeric nature of the complex in solution.Treatment of a THF solution of 1 with a stoichiometric amount of 0.3% Na/Hg amalgam resulted in a striking color change from red-black to purple. Removal of all volatile materials and recrystallization from pentane at Ϫ78°C provided dendritic, translucent, red-orange crystals. Upon [a] 2747 temperature as determined by IR and multinuclear NMR spectroscopy. The reactions of the title complex with CO, H 2 , PhSiH 3 , and its thermolysis in C 6 H 6 are reported.isolation and warming to room temperature, these crystals became purple and opaque. Repeated attempts to obtain Xray diffraction data on these purple crystals failed. However, multinuclear NMR spectroscopy and combustion analysis allowed characterization of this compound as the 16-electron species [OsBrCp*(PiPr 3 )] (2).To characterize the origin of the temperature-dependent color change associated with 2, a [D 8 ]toluene solution of 2 was cooled to Ϫ78°C under an atmosphere of nitrogen. This resulted in a color change from purple...

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“…In a later study by Donovan-Mtunzi and his team, adducts of ( 7) with group 4 and group 5 halides have been isolated and the N2 ligand properties characterized by 15 N NMR. 118 16) and ( 18)-( 21) in Table 2. In addition to the clarification of the structures of these already reported complexes, 54 this work addressed the effect of LA coordination to the N2 ligand on the 15 N NMR chemical shifts.…”

Section: Trans-[recl(n 2 )(Pme 2 Ph) 4 ] Adducts Of Early Tms Halides Complexesmentioning

confidence: 99%

Push–Pull Activation of N ₂ : Coordination of Lewis Acids to Dinitrogen Complexes

Coffinet

Simonneau

Specklin

2020

Encyclopedia of Inorganic and Bioinorganic Chemistry

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HAL is a multi-disciplinary open access archive for the deposit and dissemination of scientific research documents, whether they are published or not. The documents may come from teaching and research institutions in France or abroad, or from public or private research centers. L'archive ouverte pluridisciplinaire HAL, est destinée au dépôt et à la diffusion de documents scientifiques de niveau recherche, publiés ou non, émanant des établissements d'enseignement et de recherche français ou étrangers, des laboratoires publics ou privés.

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Nitrogen-15 nuclear magnetic resonance spectroscopy of hydrazido(2–)-, imido-, and nitrido-complexes of molybdenum and tungsten

Abstract: Nitrogen-1 5 chemical shifts and coupling constants are reported for the range of hydrazido( 2-)complexes [MX(15N15NR1R2)(dppe)2]+ (X = CI, Br, I, or HSO,; M = M o or W ; R1 = H, R2 = H, Me, or Et [and 15N2R1R2 = 15N15N(CH2)3CH2] ; dppe = Ph2PCH2CH2PPh2), [W(NCPr")(l5Nl5NH2)-

Cited by 38 publications

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Compounds of triphenylstibine and platinum: synthesis, properties and reactivity

Compounds of triphenylstibine and platinum: synthesis, properties and reactivity

Synthesis and Chemistry of the 16-Electron Osmium Complex [OsBr(η5-C5Me5)(PiPr3)]

Push–Pull Activation of N ₂ : Coordination of Lewis Acids to Dinitrogen Complexes

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Nitrogen-15 nuclear magnetic resonance spectroscopy of hydrazido(2–)-, imido-, and nitrido-complexes of molybdenum and tungsten

Abstract: Nitrogen-1 5 chemical shifts and coupling constants are reported for the range of hydrazido( 2-)complexes [MX(15N15NR1R2)(dppe)2]+ (X = CI, Br, I, or HSO,; M = M o or W ; R1 = H, R2 = H, Me, or Et [and 15N2R1R2 = 15N15N(CH2)3CH2] ; dppe = Ph2PCH2CH2PPh2), [W(NCPr")(l5Nl5NH2)-

Cited by 38 publications

References 0 publications

Compounds of triphenylstibine and platinum: synthesis, properties and reactivity

Compounds of triphenylstibine and platinum: synthesis, properties and reactivity

Synthesis and Chemistry of the 16-Electron Osmium Complex [OsBr(η5-C5Me5)(PiPr3)]

Push–Pull Activation of N 2 : Coordination of Lewis Acids to Dinitrogen Complexes

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Push–Pull Activation of N ₂ : Coordination of Lewis Acids to Dinitrogen Complexes