scholarly journals Evaluating a dispersion of sodium in sodium chloride for the synthesis of low-valent nickel complexes

2021 ◽  
Author(s):  
Elliot Johnson Humphrey ◽  
Alan Kennedy ◽  
Stephen Sproules ◽  
David Nelson
Keyword(s):  
Sodium Chloride ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Epr Spectroscopy ◽  
Nickel Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Low Valent

The use of a sodium in sodium chloride dispersion is systematically evaluated for the synthesis of nickel(0) and nickel(I) complexes from readily-prepared nickel(II) precursors. A variety of complexes with phosphine and bipyridine-type ligands were accessed, although some reactions were found to produce mixtures of nickel(0) and nickel(I), and yields were highly variable. Several new nickel(I) complexes were obtained, and these were characterised using techniques including NMR spectroscopy, EPR spectroscopy, and single crystal X-ray diffraction analysis.

scholarly journals A pyridyl-substituted cyclodisilazane [(Apy)2(μ-SiMe)2] (ApyH2 = 2-aminopyridine)

IUCrData ◽  
2017 ◽  
Vol 2 (3) ◽  
Author(s):  
Rui Li ◽  
Xin-E Duan ◽  
Wei Cao ◽  
Xue-Hong Wei
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Title Compound ◽  
Membered Ring ◽  
Side Product ◽  
Inversion Center ◽  
X Ray Diffraction ◽  
X Ray ◽  
Compound C

The title compound, C14H20N4Si2 or [(Apy)2(μ-SiMe)2], systematic name 2-[2,2,4,4-tetramethyl-3-(pyridin-2-yl)-1,3,2,4-diazadisiletidin-1-yl]pyridine, was obtained as a side product from the reaction of 2-amino-pyridine with LiBu n followed by the addition of Me2NMe2SiCl in hexane. The compound was characterized by single-crystal X-ray diffraction analysis and NMR spectroscopy. The title compound lies about an inversion center at the centroid of the cyclodisilazane ring. The four-membered Si2N2 core is strictly planar with the two pyridyl rings placed centrosymmetrically on either side of the Si2N2 plane and are almost coplanar with the central four-membered ring.

Metallaborane Reaction Chemistry. Part 3. Reaction of Carbon Monoxide with [6-H-6-(PPh3)-6P,5C-μ-(2-Ph2PC6H4)-nido-6-IrB9H12] and the Isolation and Characterisation of Two arachno-6-Monoiridadecaboranes [6-(CO)-6-H-6,9-(PPh3)2-6P,5C-μ-(2-Ph2PC6H4)-arachno-6-IrB9H11] and sym-[6-(CO)-6-H-6,6-(PMe2Ph)2-9-(PPh3)-arachno-6-IrB9H11]

1997 ◽  
Vol 62 (8) ◽  
pp. 1239-1253 ◽  
Author(s):  
Jonathan Bould ◽  
Paul Brint ◽  
John D. Kennedy ◽  
Mark Thornton-Pett ◽  
Lawrence Barton ◽  
...  
Keyword(s):  
Carbon Monoxide ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Reaction System ◽  
Structural Type ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

[6-(CO)-6-H-6,9-(PPh3)2-6P,5C-μ-(2-Ph2PC6H4)-arachno-6-IrB9H11] (1) results from the reaction of [6-H-6-(PPh3)-6P,5C-μ-(2-Ph2PC6H4)-nido-6-IrB9H12] (2) with carbon monoxide in refluxing benzene. It is characterised by NMR spectroscopy and by single-crystal X-ray diffraction analysis. Crystals were triclinic, space group P1, with a = 10.688(2), b = 13.114(3), c = 22.356(5) Å, α = 78.33(2), β = 89.482(10), γ = 70.884(12)°, and Z = 2. The compound is of the little-examined arachno ten-vertex metallaborane structural type. A second compound of this type, [6-(CO)-6-H-6,6-(PMe2Ph)2-9-(PPh3)-arachno-6-IrB9H11] (3), isolated from a reaction system involving [Ir(CO)Cl(PPh3)2], PMe2Ph and the [nido-B9H12]- anion, has also been characterised crystallographically. Crystals were triclinic, space group P1, with a = 10.389(1), b = 10.511(1), c = 19.699(3) Å, α = 75.03(1), β = 85.53(1), γ = 74.88(1)°, and Z = 2.

Eleven-Vertex Polyhedral Dicarbaplatinaborane Chemistry. Aspects of the Chemistry of Some closo-Structured {1,2,3-PtC2B8} Species and Some Related Compounds

1993 ◽  
Vol 58 (9) ◽  
pp. 2090-2120 ◽  
Author(s):  
John D. Kennedy ◽  
Bohumil Štíbr ◽  
Tomáš Jelínek ◽  
Xavier L. R. Fontaine ◽  
Mark Thornton-Pett
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
General Behaviour ◽  
Space Group ◽  
X Ray ◽  
Metal Bonding ◽  
Related Compounds

The reaction of the ten-vertex nido anions [6,9-C2B8H10]2-, [6-Me-6,9-C2B8H9]2- and [6-Ph-6,9-C2B8H9]2- with [cis-PtCl2(PMe2Ph)2] in CH2Cl2 yields the yellow crystalline closo-structured eleven-vertex compounds [2-X-1,1-(PMe2Ph)2-1,2,3-PtC2B8H9], where X = H (compound 1), Me (compound 2), or Ph (compound 3) in yields of 58 88%. These compounds have been characterized by multielement NMR spectroscopy and, in the case of compounds 1 and 2, by single-crystal X-ray diffraction analysis. Crystals of compound 1 were monoclinic, space group P21/n, with a = 947.6(1), b = 1 547.7(3), c = 1 804.0(3) pm, β = 104.78(1)°, and Z = 4, solved and refined to R (Rw) = 0.0216 (0.0234) with 4 200 unique reflections I > 2.0 σ(I). Crystals of compound 2 were monoclinic, space group I2/a (= C2/c), with a = 1 824.8(2), b = 1 016.8(2), c = 1 328.2(3) pm, β = 101.48(2)°, and Z = 4, solved and refined to R (Rw) = 0.0442 (0.0474) with 2 057 unique reflections I > 2.0 σ(I). The NMR and X-ray results reveal that the closed eleven-vertex compounds [2-X-1,1-(PR3)2-1,2,3-PtC2B8H9] exhibit a previously unsuspected but very free contrarotational fluxionality within the constrains of their η6-carborane-to-metal bonding that is accompanied by a marked flexing of the η6-{C2B8H9X} moiety between nido and arachno ten-vertex geometries and electronic characteristics. The structural and bonding implications are discussed and elucidated specifically with reference to the NMR and geometrical charcteristics of [closo-2,3- C2B9H11], [arachno-6,9- C2B8H14] and the [nido-6-X-6,9- C2B8H9]2- anions, together with other pertinent species such as [μ-6,9-(SnMe2)-nido-6,9-C2B8H10] and more generally with reference to other eleven-vertex metallaheteroborano species. The general behaviour patterns thus established are summarized.

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.

Ten-Vertex Polyhedral Monocarbaborane Chemistry. The Novel High-Yield Formation of the Ten-Vertex closo Compound [6-(PMe2Ph)-closo-1-CB9H9] from the Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11]

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
High Yield ◽  
Monoclinic Space Group ◽  
The Novel ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
X Ray ◽  
Yield Formation ◽  
Boiling Toluene

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.

Synthesis of 4-(3-coumarinyl)-3-benzyl-4-thiazolin-2-one 4-methylbenzylidenehydrazone and determination of the isomeric structure by X-ray analysis

2003 ◽  
Vol 218 (12) ◽  
Author(s):  
Süheyla Özbey ◽  
Nilgün Karalı ◽  
Aysel Gürsoy
Keyword(s):  
Single Crystal ◽  
Diffraction Analysis ◽  
Spectral Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Isomeric Structure ◽  
Elemental Analyses

AbstractIn this study 4-(3-coumarinyl)-3-benzyl-4-thi azolin-2-one 4-methylbenzylidenehydrazone 3 was synthesised. An independent proof of the thiazolylhydrazone structure of 3 was achieved by single crystal X-ray diffraction analysis. Elemental analyses and spectral data (IR,

Single-crystal X-ray diffraction analysis of nonplanar autoepitaxial silicon layers

2009 ◽  
Vol 45 (14) ◽  
pp. 1610-1613
Author(s):  
V. T. Bublik ◽  
L. V. Kozhitov ◽  
T. T. Kondratenko
Keyword(s):  
Single Crystal ◽  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
X Ray

An Intramolecular Boron Nitrogen Lewis Acid Base Pair on a Rigid Naphthyl Backbone

2012 ◽  
Vol 67 (6) ◽  
pp. 589-593 ◽  
Author(s):  
Daniel Winkelhaus ◽  
Beate Neumann ◽  
Norbert W. Mitzel
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Lewis Acid ◽  
Elemental Analysis ◽  
Base Pair ◽  
Ring System ◽  
X Ray Diffraction ◽  
Acid Base ◽  
X Ray ◽  
Boron Nitrogen

The reaction of (C6F5)2BCl with 8-lithio-N,N-dimethyl-1-naphthylamine (1) afforded the fivemembered ring system 8-bis(pentafluorophenyl)boryl-N,N-dimethyl-1-naphthylamine (2) with an intramolecular dative B-N bond. The compound was characterised by elemental analysis, NMR spectroscopy and single-crystal X-ray diffraction.

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