Insertion of Chalcogens and Bis(tert-butylisonitrile)palladium(0) into a Strained Ruthenium Half-sandwich Complex

2012 ◽  
Vol 67 (11) ◽  
pp. 1173-1177 ◽  
Author(s):  
Holger Braunschweig ◽  
Alexander Damme ◽  
Jan Mies ◽  
Marius Schäfer
Keyword(s):  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
Sandwich Complex ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Multinuclear Nmr Spectroscopy ◽  
Group 16 ◽  
Half Sandwich

The previously synthesized strained distannadiyl-ansa half-sandwich complex [{k1-SntBu2- SntBu2-(η5-C5H5)}Ru(CO)2] was investigated with respect to its reactivity toward group 16 elements and bis(tert-butylisonitrile)palladium(0). All products were analyzed by multinuclear NMR spectroscopy, IR spectroscopy and elemental analysis. [{k1-SntBu2SSntBu2-(η5-C5H5)}Ru(CO)2] was furthermore characterized by X-ray diffraction.

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.

Synthesis of Sterically Demanding Bis(phosphinimine) Dibenzofuran Ligands and Subsequent Zinc Metalation

2015 ◽  
Vol 68 (3) ◽  
pp. 373 ◽  
Author(s):  
Matthew T. Zamora ◽  
Saif M. Zahir ◽  
Kevin R. D. Johnson ◽  
Clay J. Barnson ◽  
Craig A. Wheaton ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Ambient Temperature ◽  
Elemental Analysis ◽  
Elimination Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Sterically Demanding ◽  
Multinuclear Nmr Spectroscopy ◽  
Alkane Elimination

In light of previous success surrounding the use of bis(phosphinimine)dibenzofuran ligands for zinc-mediated lactide polymerization, a series of sterically demanding P=N pincer compounds have been prepared with important steric and electronic modifications at both P- and N-sites (L, 3a–d). These systems are highly crystalline and have been extensively characterized using multinuclear NMR spectroscopy, elemental analysis, and X-ray diffraction. The ligands can be transformed into their protonated analogues [HL][BArF4] (4a–d, [BArF4] = [B(m-(CF3)2-C6H3)4]) by reaction with Brookhart’s acid, and subsequently coordinated to zinc via an alkane elimination reaction with [ZnEt2] at ambient temperature to afford the corresponding [LZnEt][BArF4] cationic complexes 5a–d. In addition, an unusual chloridozinc species [LZnCl][BArF4] (5c′) has been isolated and structurally characterized, providing comparisons to previously established ligand sets with similar geometries.

Dimethyl Sulfate Induced Nucleophilic Substitution of the [Bis(1,2-dicarbollido)-3-cobalt(1-)]ate Ion. Syntheses, Properties and Structures of Its 8,8'-μ-Sulfato, 8-Phenyland 8-Dioxane Derivatives

1997 ◽  
Vol 62 (1) ◽  
pp. 47-56 ◽  
Author(s):  
Jaromír Plešek ◽  
Stanislav Heřmánek ◽  
Andreas Franken ◽  
Ivana Císařová ◽  
Christiane Nachtigal
Keyword(s):  
Nmr Spectroscopy ◽  
Nucleophilic Substitution ◽  
Acid Catalysis ◽  
Dimethyl Sulfate ◽  
General Mechanism ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Multinuclear Nmr Spectroscopy

Syntheses and structures of [8,8'-μ-(OSO2O)(1,2-C2B9H10)2-3-Co]-and [(8-Ph-1,2-C2B9H10)-3-Co-(1',2'-C2B9H11]- ions and of [(8-dioxane-1,2-C2B9H10)-3-Co-(1',2'-C2B9H11)] zwitterion are described. All compounds result on dimethyl sulfate induced nucleophilic B-substitution of the parent cobalta-carborane sandwich ion under acid catalysis. A general mechanism is proposed. Constitutions of all compounds are inferred from the mass and multinuclear NMR spectroscopy and all structures are established by X-ray diffraction. Selected NMR and X-ray data are presented.

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 =...

Exploring the Anion–Cation Interaction inm-Terphenyltetrafluorosilicates by Using Multinuclear NMR Spectroscopy, X-ray Diffraction, and ICR-FT-MS

2009 ◽  
Vol 15 (37) ◽  
pp. 9521-9529 ◽  
Author(s):  
Stefan Spirk ◽  
Ferdinand Belaj ◽  
Martin Nieger ◽  
Harald Köfeler ◽  
Gerald N. Rechberger ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Multinuclear Nmr Spectroscopy

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.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

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