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.

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 of O-aminoalkyl derivatives of 7-hydroxy-4-methylcoumarin by 13C CP/MAS NMR and X-ray diffraction methods

2011 ◽  
Vol 998 (1-3) ◽  
pp. 42-48 ◽  
Author(s):  
Joanna Trykowska Konc ◽  
Elżbieta Hejchman ◽  
Dorota Maciejewska ◽  
Irena Wolska
Keyword(s):  
Solid State ◽  
Mas Nmr ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Cp Mas Nmr ◽  
Derivatives Of ◽  
13C Cp Mas Nmr

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.

Phosphine chalcogenide complexes of antimony(III) halides

2015 ◽  
Vol 93 (3) ◽  
pp. 375-379 ◽  
Author(s):  
Karlee L. Bamford ◽  
Alasdair P.M. Robertson ◽  
Hilary A. Jenkins ◽  
Brian O. Patrick ◽  
Neil Burford
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Phosphine Oxide ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Derivatives Of

Three series of phosphine chalcogenide complexes of the antimony(III) halides SbX3 (X = F, Cl, Br, or I) have been synthesized and characterized by spectroscopic and crystallographic methods. Complexes of the generic formulae (Cy3PO)SbX3 (X = F (1a), Cl (1b), or Br (1c)), (Cy3PO)2SbX3 (X = F (2a), Cl (2b), or Br (2c)), and (Cy3PS)SbX3 (X = Cl (3b), Br (3c), or I (3d)) were synthesized via the treatment of solutions of SbX3 with OPCy3 and SPCy3, respectively. Derivatives of (Cy3PO)SbX3 were characterized by single crystal X-ray diffraction for 1a and 1b and crystallize as dimers through symmetry related intermolecular Sb–X interactions, providing the first structurally characterized examples of this class of complex. Derivatives of (Cy3PS)SbX3 (3b–3c) adopt analogous dimeric structures in the solid state. The solid-state structure of (Cy3PO)2SbCl3 (2b) is consistent with the previously reported structures of bis-phosphine oxide complexes of antimony(III), with a square pyramidal Sb center and cis-configured OPCy3 ligands. The phosphine chalcogenide complexes of SbX3 display configurations that are consistent with the perceived trans-labilizing properties of the ligands/substituents.

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.

Solid-state structure and solution conformation of 2,2,4,4,6,6,-hexa-(p-chlorophenoxo)cyclotri-λ5-phosphazatriene. X-Ray and dipole moment studies

1989 ◽  
pp. 757-760 ◽  
Author(s):  
Giuliano Bandoli ◽  
Umberto Casellato ◽  
Mario Gleria ◽  
Antonio Grassi ◽  
Enzo Montoneri ◽  
...  
Keyword(s):  
Dipole Moment ◽  
Solid State ◽  
State Structure ◽  
Solution Conformation ◽  
Solid State Structure ◽  
X Ray

The solid state structure and environmental polarization effect of a novel asymmetric azine

2017 ◽  
Vol 41 (19) ◽  
pp. 11361-11371 ◽  
Author(s):  
Clodoaldo Valverde ◽  
Wesley F. Vaz ◽  
Jean M. F. Custodio ◽  
Vitor S. Duarte ◽  
Paulo S. Carvalho-Jr ◽  
...  
Keyword(s):  
Solid State ◽  
Polarization Effect ◽  
State Structure ◽  
Solid State Structure ◽  
Solid State Characterization

Extensive solid state characterization of a novel asymmetric azine and its environmental polarization effect is reported.

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