Synthesis of Stabilized Phosphinidenoid Complexes Using Weakly Coordinating Cations

2011 ◽  
Vol 64 (12) ◽  
pp. 1583 ◽  
Author(s):  
Lili Duan ◽  
Vitaly Nesterov ◽  
Jason W. Runyon ◽  
Gregor Schnakenburg ◽  
Anthony J. Arduengo III ◽  
...  
Keyword(s):  
Thermal Stability ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Tert Butyl ◽  
Multinuclear Nmr Spectroscopy ◽  
Complex Salts ◽  
Weakly Coordinating ◽  
Thermal Stability Of

The formation of phosphinidenoid complex salts having weakly coordinating cations (WCCs) is reported via treatment of P-functional phosphane complexes with N,N’-di-tert-butyl imidazol-2-ylidene or a P4-t-Bu phosphazene base. The thermal stability of phosphinidenoid complex salts is dependent upon the P–X substituents and the nature of the WCC. The complexes were characterized by multinuclear NMR spectroscopy and confirmed by single-crystal X-ray structure.

scholarly journals Ring opening polymerisation of L and rac lactide using group 4 permethylpentalene aryloxides and alkoxides

2021 ◽  
Author(s):  
Zoe Turner ◽  
Jessica Lamb ◽  
Thomas Robinson ◽  
Dipa Mandal ◽  
Jean-Charles Buffet ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Ring Opening ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
New Family ◽  
Group 4 ◽  
Multinuclear Nmr Spectroscopy

A new family of group 4 permethylpentalene (C8Me62–; Pn*) aryloxide and alkoxide complexes have been synthesised and fully characterised by multinuclear NMR spectroscopy and single-crystal X-ray diffraction; (η8-C8Me6)Zr(OR)2 (R =...

Pentafluorophenyl and phenyl substituted azidoborates

2002 ◽  
Vol 80 (11) ◽  
pp. 1444-1450 ◽  
Author(s):  
Wolfgang Fraenk ◽  
Thomas M Klapötke ◽  
Burkhard Krumm ◽  
Heinrich Nöth ◽  
Max Suter ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Boron Atom ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
X Ray Crystallography ◽  
Multinuclear Nmr Spectroscopy

The azidoborates [(C6F5)4–nB(N3)n]– (n = 1–3) (1–3) were synthesized by reacting the corresponding borane with [R]N3 (R = Me4N, Ph4P). To study the influence of the electron withdrawing C6F5-substituent on the boron atom, [Me4N][(C6H5)3BN3] (4) was also prepared. All compounds were fully characterized by IR, Raman, and multinuclear NMR spectroscopy in addition to characterization by single crystal diffraction analyses.Key words: azidoborate, pentafluorophenyl, multinuclear NMR spectroscopy, X-ray crystallography.

Hungry for charge – how a beryllium scorpionate complex “eats” a weakly coordinating anion

2020 ◽  
Vol 75 (5) ◽  
pp. 503-508
Author(s):  
Dominik Naglav-Hansen ◽  
Kevin Dzialkowski ◽  
Briac Tobey ◽  
Christoph Wölper ◽  
Georg Jansen ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Quantum Chemical Calculations ◽  
Quantum Chemical ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr Spectroscopy ◽  
Weakly Coordinating ◽  
Weakly Coordinating Anion ◽  
Heteroleptic Complex

AbstractWe present the reaction of a tris(pyrazolyl) beryllium scorpionate (TpBe) complex with a weakly coordinating anion (WCA), which yields the heteroleptic complex TpBeOC(CF3)31 (TpBeORF). The product 1 has been characterized by multinuclear NMR spectroscopy (1H, 9Be, 13C) and single-crystal X-ray diffraction (scXRD). Quantum chemical calculations (DFT, NPA, LOL) were performed to study the bonding nature in 1.

scholarly journals Half-Sandwich Arene-Osmium(II) Complexes with Phosphinite Ligands

Molbank ◽  
10.3390/m1110 ◽  
2020 ◽  
Vol 2020 (1) ◽  
pp. M1110 ◽  
Author(s):  
Rebeca González-Fernández ◽  
Javier Borge ◽  
Pascale Crochet ◽  
Victorio Cadierno
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Study ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Intramolecular Exchange ◽  
Multinuclear Nmr Spectroscopy ◽  
Half Sandwich

The synthesis of a series of arene-osmium(II) complexes containing phosphinite-type ligands, namely, [OsCl2(η6-p-cymene){R2PO(CH2)nPh}] (R = Ph, n = 1 (4a), 2 (4b), 3 (4c); R = iPr, n = 1 (5a), 2 (5b), 3 (5c)) and [OsCl2(η6-benzene){iPr2PO(CH2)2Ph}] (7), is presented. All these compounds were characterized by elemental analysis and multinuclear NMR spectroscopy (31P{1H}, 1H and 13C{1H}), and the structure of [OsCl2(η6-p-cymene){Ph2PO(CH2)3Ph}] (4c) unequivocally confirmed through a single-crystal X-ray diffraction study. Attempts to generate the tethered species [OsCl2{η6:κ1(P)-C6H5(CH2)nOPR2}] by intramolecular exchange of the coordinated arene in 4-5a-c or 7, upon thermal or MW heating, failed.

Unusual Rearrangement of Naphthalene in the Synthesis of a Novel B8-B8-Bridged Derivative in the [(1,2-C2B9H11)2-3-Co]- Series. X-Ray Structure and 11B NMR Spectra of [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- (CH3)4N+

1997 ◽  
Vol 62 (5) ◽  
pp. 746-751 ◽  
Author(s):  
Andreas Franken ◽  
Jaromír Plešek ◽  
Christiane Nachtigal
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Nucleophilic Substitution ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Unusual Rearrangement ◽  
Multinuclear Nmr Spectroscopy ◽  
11B Nmr ◽  
Isolated Compound

On treatment of the [(1,2-C2B9H11)2Co]- ion with naphthalene in presence of AlCl3 a remarkably bridged [8,8'-μ-(CH2-C9H6)-(1,2-C2B9H10)2-3-Co]- ion is obtained as a single isolated compound. The triatomic -CH2-C9H6- bridge is derived from the rearranged naphthalene nucleus. The mechanism of this reaction is obscure but it does resemble the "Electrophile-Induced Nucleophilic Substitution" reported earlier. The structure of the compound was established by multinuclear NMR spectroscopy and by single crystal X-ray diffraction.

Polymorphism of Potassium Ferrocyanide Trihydrate as Studied by Solid-State Multinuclear NMR Spectroscopy and X-ray Diffraction

2009 ◽  
Vol 48 (10) ◽  
pp. 4342-4353 ◽  
Author(s):  
Mathew J. Willans ◽  
Roderick E. Wasylishen ◽  
Robert McDonald
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Potassium Ferrocyanide ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Multinuclear Nmr Spectroscopy ◽  
Potassium Ferrocyanide Trihydrate

Thermal Stability of CoSi2 on Single Crystal and Polycrystalline Silicon

1990 ◽  
Vol 182 ◽  
Author(s):  
J. R. Phillips ◽  
P. Revesz ◽  
J. O. Olowolafe ◽  
J. W. Mayer
Keyword(s):  
Electron Microscopy ◽  
Thermal Stability ◽  
Single Crystal ◽  
Polycrystalline Silicon ◽  
Sheet Resistivity ◽  
X Ray ◽  
Resistivity Measurements ◽  
Silicide Layer ◽  
Thermal Stability Of ◽  
Scanning Electron

AbstractThe thermal stability of Co silicide on single crystal and polycrystalline Si has been investigated. Co films were evaporated onto (100) Si and undoped polycrystalline Si and annealed in vacuum. Resulting silicide films were examined using Rutherford backscattering spectroscopy, scanning electron microscopy, electron—induced x—ray spectroscopy, and sheet resistivity measurements. We find that CoSi2 on single crystal (100) Si remains stable through 1000ºC. In contact with undoped polycrystalline Si, intermixing begins at temperatures as low as 650ºC for 30min annealing. The Co silicide and Si layers are intermixed after 750ºC 30min annealing, giving islands of Si surrounded by silicide material, with both components extending from the surface down to the underlying oxide layer. The behavior of CoSi2 contrasts with results reported for TiSi2 which agglomerates on single crystal Si around 900ºC but is stable on polycrystalline silicon as high as 800ºC. Resistivity measurements show that the Co silicide remained interconnected despite massive incursion by Si into the silicide layer.

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