scholarly journals Taking Advantage of Ortho- and Peri-Substitution to Design Original 9-Membered P,O,Si-Heterocycles

2021 ◽  
Author(s):  
Thomas Delouche ◽  
Elsa Caytan ◽  
Cassandre Quinton ◽  
Thierry Roisnel ◽  
Marie Cordier ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Analysis ◽  
Synthetic Method ◽  
Phosphine Oxides ◽  
X Ray ◽  
Detailed Structural Analysis

A family of 9 cyclic phosphine-disiloxane featuring peri-substituted naphthyl(Nap)/acenaphthyl(Ace) scaffolds have been prepared and fully characterized including X-ray structure, which allows a detailed structural analysis. This straightforward synthesis takes advantage of both ortho- and peri-substitution of Nap/Ace-substituted phosphine oxides. The synthetic method allows diversifying the polyaromatic platform (Nap and Ace) as well as the Si substituents (Me and Ph). Despite a strong steric congestion, the P-atom remains reactive toward oxidation or coordination. In particular, Au(I) complex could be prepared. All the compounds display absorption/luminescence in the UV-Vis range. Surprisingly, the P-trivalent derivatives display unexpected luminescence in the green in solid-state.

scholarly journals Taking Advantage of Ortho- and Peri-Substitution to Design Original 9-Membered P,O,Si-Heterocycles

2021 ◽  
Author(s):  
Thomas Delouche ◽  
Elsa Caytan ◽  
Cassandre Quinton ◽  
Thierry Roisnel ◽  
Marie Cordier ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Analysis ◽  
Synthetic Method ◽  
Phosphine Oxides ◽  
X Ray ◽  
Detailed Structural Analysis

A family of 9 cyclic phosphine-disiloxane featuring peri-substituted naphthyl(Nap)/acenaphthyl(Ace) scaffolds have been prepared and fully characterized including X-ray structure, which allows a detailed structural analysis. This straightforward synthesis takes advantage of both ortho- and peri-substitution of Nap/Ace-substituted phosphine oxides. The synthetic method allows diversifying the polyaromatic platform (Nap and Ace) as well as the Si substituents (Me and Ph). Despite a strong steric congestion, the P-atom remains reactive toward oxidation or coordination. In particular, Au(I) complex could be prepared. All the compounds display absorption/luminescence in the UV-Vis range. Surprisingly, the P-trivalent derivatives display unexpected luminescence in the green in solid-state.

A bis-Au(III) [28]hexaphyrin triphenylphosphine adduct

2016 ◽  
Vol 20 (08n11) ◽  
pp. 997-1001 ◽  
Author(s):  
Koji Naoda ◽  
Atsuhiro Osuka
Keyword(s):  
Solid State ◽  
Structural Analysis ◽  
Trifluoroacetic Acid ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
X Ray ◽  
H Nmr ◽  
Detailed Structural Analysis ◽  
Nir Absorption ◽  
Plausible Mechanism

Triphenylphosphine was added regioselectively at the C(3) position of bis-Au(III) complex of [26]hexaphyrin 5 in the presence of trifluoroacetic acid to produce [28]hexaphyrin triphenylphosphine adduct 6 in 62% yield, which has been fully characterized by NMR, UV-vis/NIR absorption, and MS spectroscopies, and X-ray diffraction analysis. The rigid planar structure forces 6 to take Hückel antiaromaticity, which has been supported by its 1H NMR spectrum. Curiously, the detailed structural analysis elucidated that the triphenylphosphine moiety exists as a phosphorane form in the solid state. A plausible mechanism via a double protonated 5 is proposed, which can explain the observed regioselectivity.

Chiral Sulfur Compounds. XVIII. Structure and Conformation of Methyl (E,S*)-3-Phenyl-2-(phenylsulfinyl)propenoate

1992 ◽  
Vol 45 (11) ◽  
pp. 1923 ◽  
Author(s):  
KA Hellmund ◽  
SG Pyne ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Circular Dichroism ◽  
Solid State ◽  
Structural Analysis ◽  
Title Compound ◽  
Sulfur Compounds ◽  
Methanol Solution ◽  
X Ray ◽  
Circular Dichroïsm

The X-ray structural analysis of the title compound shows that the s-cis conformation is favoured in the solid state. This conformation is consistent with circular dichroism studies in methanol solution.

scholarly journals Structural Analysis of a Melaminium Polyphosphate from X-ray Powder Diffraction and Solid-State NMR Data

2005 ◽  
Vol 109 (28) ◽  
pp. 13529-13537 ◽  
Author(s):  
Vladimir Brodski ◽  
René Peschar ◽  
Henk Schenk ◽  
Andreas Brinkmann ◽  
Tom G. Bloemberg ◽  
...  
Keyword(s):  
Solid State ◽  
Structural Analysis ◽  
Powder Diffraction ◽  
Solid State Nmr ◽  
X Ray ◽  
Nmr Data

scholarly journals Building solids inside nano-space: from confined amorphous through confined solvate to confined ‘metastable’ polymorph

2015 ◽  
Vol 17 (38) ◽  
pp. 24761-24773 ◽  
Author(s):  
K. P. Nartowski ◽  
J. Tedder ◽  
D. E. Braun ◽  
L. Fábián ◽  
Y. Z. Khimyak
Keyword(s):  
Solid State ◽  
Structural Analysis ◽  
Mesoporous Silicas ◽  
Detailed Structural Analysis ◽  
Pharmaceutical Molecules

The detailed structural analysis and the control of solid state transformations of encapsulated pharmaceutical molecules inside the pores of mesoporous silicas are demonstrated.

scholarly journals Selective Hydration of Nitriles to Corresponding Amides in Air with Rh(I)-N-Heterocyclic Complex Catalysts

Catalysts ◽  
2020 ◽  
Vol 10 (1) ◽  
pp. 125 ◽  
Author(s):  
Csilla Enikő Czégéni ◽  
Sourav De ◽  
Antal Udvardy ◽  
Nóra Judit Derzsi ◽  
Gergely Papp ◽  
...  
Keyword(s):  
Catalytic Activity ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Catalytic Properties ◽  
13C Nmr Spectroscopy ◽  
Synthetic Method ◽  
X Ray Diffraction ◽  
Nitrile Hydration ◽  
X Ray

A new synthetic method for obtaining [RhCl(cod)(NHC)] complexes (1–4) (cod = η4-1,5-cyclooctadiene, NHC = N-heterocyclic carbene: IMes, SIMes, IPr, and SIPr, respectively) is reported together with the catalytic properties of 1–4 in nitrile hydration. In addition to the characterization of 1–4 in solution by 13C NMR spectroscopy, the structures of complexes 3, and 4 have been established also in the solid state with single-crystal X-ray diffraction analysis. The Rh(I)-NHC complexes displayed excellent catalytic activity in hydration of aromatic nitriles (up to TOF = 276 h−1) in water/2-propanol (1/1 v/v) mixtures in air.

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