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.

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 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 =...

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.

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.

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

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.

scholarly journals Reactions of Dihaloboranes with Electron-Rich 1,4-Bis(trimethylsilyl)-1,4-diaza-2,5-cyclohexadienes

Molecules ◽  
2020 ◽  
Vol 25 (12) ◽  
pp. 2875
Author(s):  
Li Ma ◽  
Xiaolin Zhang ◽  
Wenbo Ming ◽  
Shengxin Su ◽  
Xiaoyong Chang ◽  
...  
Keyword(s):  
Double Bond ◽  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
1H Nmr Spectroscopy ◽  
Variable Temperature ◽  
Organosilicon Compounds ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr Spectroscopy ◽  
Bond Character

The reactions of electron-rich organosilicon compounds 1,4-bis(trimethylsilyl)-1,4-diaza-2,5-cyclohexadiene (1), 2,3,5,6-tetramethyl-1,4-bis(trimethylsilyl)-1,4-diaza-2,5-cyclohexadiene (2), and 1,1′-bis(trimethylsilyl)-1,1′-dihydro-4,4′-bipyridine (12) with B-amino and B-aryl dihaloboranes afforded a series of novel B=N-bond-containing compounds 3–11 and 13. The B=N rotational barriers of 7 (>71.56 kJ/mol), 10 (58.79 kJ/mol), and 13 (58.65 kJ/mol) were determined by variable-temperature 1H-NMR spectroscopy, thus reflecting different degrees of B=N double bond character in the corresponding compounds. In addition, ring external olefin isomers 11 were obtained by a reaction between 2 and DurBBr2. All obtained B=N-containing products were characterized by multinuclear NMR spectroscopy. Compounds 5, 9, 10a, 11, and 13a were also characterized by single-crystal X-ray diffraction analysis.

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