Vanadium and niobium diamidophosphine complexes and their reactivity

2003 ◽  
Vol 81 (12) ◽  
pp. 1431-1437 ◽  
Author(s):  
Michael P Shaver ◽  
Robert K Thomson ◽  
Brian O Patrick ◽  
Michael D Fryzuk
Keyword(s):  
Coordination Chemistry ◽  
Solid State ◽  
Molecular Nitrogen ◽  
Tridentate Ligand ◽  
State Structure ◽  
Butyl Lithium ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Unstable Complex

The tridentate ligand precursors R′P(CH2SiMe2NR′′)2 (R′R′′[NPN]: R′ = Cy, Ph; R′′ = Ph, Mes, Me) were prepared from metathesis reactions of a lithiated amine, chloro(chloromethyl)dimethylsilane, the appropriate 1° phosphine, and n-butyl lithium and were isolated as solvent adducts. Metathesis between CyPh[NPN]Li2(OEt2), 2, and VCl3(THF)3 afforded (CyPh[NPN]VCl)2, 7, whose solid-state structure was established by X-ray crystallography. Reduction attempts of the (R′R′′[NPN]VCl)2 species with KC8 incorporated molecular nitrogen but were complicated by imide formation and ligand decomposition. Metathesis of 2 with NbCl2Me3 afforded the highly unstable complex CyPh[NPN]NbMe3, 15. Attempts to hydrogenate this species were unsuccessful.Key words: vanadium, niobium, metathesis, coordination chemistry, reduction, hydrogenation.

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

Solid-state structure of NH-pyrazolium hydrochlorides and hydrobromides by X-ray crystallography and CPMAS NMR

1997 ◽  
Vol 415 (1-2) ◽  
pp. 81-92 ◽  
Author(s):  
Concepción Foces-Foces ◽  
Lourdes Infantes ◽  
Rosa Marı́a Claramunt ◽  
Concepción López ◽  
Nadine Jagerovic ◽  
...  
Keyword(s):  
Solid State ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

Solid-State Structure and Tautomerism of 2-Aminotroponimines Studied by X-ray Crystallography and Multinuclear NMR Spectroscopy

2004 ◽  
Vol 2004 (21) ◽  
pp. 4452-4466 ◽  
Author(s):  
Rosa M. Claramunt ◽  
Dionisia Sanz ◽  
Marta Pérez-Torralba ◽  
Elena Pinilla ◽  
M. Rosario Torres ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
Multinuclear Nmr ◽  
X Ray Crystallography ◽  
Multinuclear Nmr Spectroscopy

Ionic versus Covalent Bonding in Dilithium Porphyrins: X-ray Structure of Dilithium Tetraphenylporphyrin Bis(etherate)

1997 ◽  
Vol 01 (02) ◽  
pp. 121-124 ◽  
Author(s):  
DENISHA Y. DAWSON ◽  
JOHN ARNOLD
Keyword(s):  
Solid State ◽  
Diethyl Ether ◽  
Covalent Bonding ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The solid state structure of dilithium tetraphenylporphyrin bis(etherate) has been determined by X-ray crystallography. The structure shows the lithium atoms are displaced out of the plane of the porphyrin, each coordinated in a square pyramidal fashion to the four nitrogen atoms in addition to a molecule of diethyl ether. The lithium atoms are identical, as required by the crystallographic inversion centre. X-ray data are as follows: [Formula: see text] (# 2) with a = 10.1908(4) Å, b = 11.6553(4) Å, c = 12.5199(5) Å, α = 111.644(1)°, β = 98.029(1)°, γ = 111.883(1)°, V = 1214.61(9)Å3, dcalc = 1.171 g cm -3 and Z = 1.

Oxide, Sulfide, Selenide, and Borane Derivatives of Indenylphosphines

2003 ◽  
Vol 56 (11) ◽  
pp. 1153 ◽  
Author(s):  
Julian J. Adams ◽  
David E. Berry ◽  
Owen J. Curnow ◽  
Glen M. Fern ◽  
Michelle L. Hamilton ◽  
...  
Keyword(s):  
Solid State ◽  
13C Nmr Spectroscopy ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Isolation And Characterization ◽  
Linear Relationships ◽  
Derivatives Of

We report the preparation, isolation and characterization of oxide, sulfide, selenide, and borane derivatives of a series of indenylphosphines. Some members of the series had already been prepared, and we have completed the series. We have prepared (indenyl)xPh3-xPO (x = 1–3) for the oxide series, (indenyl)xPh3-xPS (x = 3) for the sulfides, (indenyl)xPh3-xPSe (x = 1,2) for the selenides, and (indenyl)xPh3-xPBH3 (x = 1–3) for the boranes. Linear relationships of the 31P NMR chemical shift with the number of indenyl groups were observed. The compounds were also characterized by 1H and 13C NMR spectroscopy and mass spectrometry. The solid-state structure of diindenylphenylphosphine selenide was determined by X-ray crystallography and found to be isomorphous with diindenylphenylphosphine sulfide. The solid-state structure of triindenylphosphine sulfide was also determined by X-ray crystallography and the indenyl groups were confirmed to all be the inden-3-yl isomer. Additionally, pentacarbonyl(triindenylphosphine)molybdenum(0), 1,3-bis(diphenylphosphino)indene diborane, and rac-bis(1-(diphenylphosphino)indenyl)ironII) diborane were prepared, isolated, and characterized.

Structural Study of an Acyclic Diterpene From Eremophila Species

1996 ◽  
Vol 49 (6) ◽  
pp. 701 ◽  
Author(s):  
YM Syah ◽  
EL Ghisalberti ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Structural Study ◽  
Room Temperature ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of the semicarbazone derivative (3) of the aldehyde diacid (1), an acyclic diterpene isolated from Eremophila species, has been determined by a single-crystal room-temperature X-ray study. Crystals of (3) are triclinic, Pī , a 14.642(7), b 14.371(6), c 12.823(6) Ǻ, α 76.59(4), β 66.09(4), γ 72.97(4)°, Z = 4; R was 0.052 for 2265 independent 'observed' (I > 3σ(I)) diffractometer reflections.

N–O Bond Cleavage During the Deprotonation of N,O-Bis(trimethylsilyl)hydroxylamine

2008 ◽  
Vol 63 (3) ◽  
pp. 339-341 ◽  
Author(s):  
Ajay Venugopal ◽  
Alexander Willner ◽  
Norbert W. Mitzel
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Bond Cleavage ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Potassium Hydride ◽  
Oxygen Atoms

The reaction of N,O-bis(trimethylsilyl)hydroxylamine with potassium hydride in pentane affords a product of the formula {K6[OSiMe3]4[ON(SiMe3)2]2}, resulting from deprotonation followed by N-O bond cleavage and 1,2-silylshift. The compound was characterised by elemental analysis and by single crystal X-ray diffraction. The aggregate consists of a K3O3 bis-cubane core, with N(SiMe3)2 groups at the oxygen atoms shared by the two cubes, andMe3Si groups attached to the four O vertices. Two weak K···N interactions are also detected in the solid state structure.

Notizen: Solid State Structure of N,N-Dibenzylhydroxylamine

1995 ◽  
Vol 50 (4) ◽  
pp. 699-701 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Jürgen Riede ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of N,N-dibenzylhydroxylamine (1) has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P 21/n with four formula units in the unit cell. N,N-dibenzylhydroxylamine dimerizes to give N2O2H2 sixmembered rings as a result of the formation of two hydrogen bonds O - H ··· N in the solid state.

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