scholarly journals Synthesis and Characterization of Cyclic Silenolates

2014 ◽  
Author(s):  
Michael Haas ◽  
Roland Fischer ◽  
Ana Torvisco ◽  
Harald Stueger
Keyword(s):  
Single Crystals ◽  
Structure Analysis ◽  
High Selectivity ◽  
Ring Cleavage ◽  
Synthesis And Characterization ◽  
Nmr Analysis ◽  
Subsequent Reaction ◽  
X Ray ◽  
Carbonyl Function

Based on earlier work by Ottosson [1] and Ohshita [2] the previously unknown cyclic silenolates 1a-c and 2a-b have been synthesized by the reaction of acylcyclohexasilanes with one or two equivalents of KOtBu. The nature of the anions (silenide or silenolate) and consequently the outcome of subsequent reaction steps largely depends on the substituent R at the carbonyl function. Detailed NMR-analysis of 1a-c and 2a-b corroborate this deduction. Furthermore, for 1a-c and 2a-b single crystals which were suitable for X-ray structure analysis could be grown. Very interesting is the reactivity of 1b, which at 50°C undergoes a hitherto unknown 1,4-trimethylsilyl-migration followed by a ring cleavage of the cyclohexasilane cycle to form the anion 3a. The high selectivity of these reactions is demonstrated by the formation of an acyl-functionalized bicyclo-2,2,2-octasilane in >90% yield from 2a and \(ClSiMe_{2}SiMe_{2}Cl\).

scholarly journals Arene Ruthenium Metalla-Assemblies with Anthracene Moieties for PDT Applications

Inorganics ◽  
2018 ◽  
Vol 6 (3) ◽  
pp. 97 ◽  
Author(s):  
Marie Gaschard ◽  
Farzaneh Nehzat ◽  
Thomas Cheminel ◽  
Bruno Therrien
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
General Formula ◽  
Structure Analysis ◽  
White Light ◽  
Light Irradiation ◽  
Synthesis And Characterization ◽  
X Ray

The synthesis and characterization of three metalla-rectangles of the general formula [Ru4(η6-p-cymene)4(μ4-clip)2(μ2-Lanthr)2][CF3SO3]4 (Lanthr: 9,10-bis(3,3’-ethynylpyridyl) anthracene; clip = oxa: oxalato; dobq: 2,5-dioxido-1,4-benzoquinonato; donq: 5,8-dioxido-1,4-naphthoquinonato) are presented. The molecular structure of the metalla-rectangle [Ru4(η6-p-cymene)4(μ4-oxa)2(μ2-Lanthr)2]4+ has been confirmed by the single-crystal X-ray structure analysis of [Ru4(η6-p-cymene)4(μ4-oxa)2(μ2-Lanthr)2][CF3SO3]4 · 4 acetone (A2 · 4 acetone), thus showing the anthracene moieties to be available for reaction with oxygen. While the formation of the endoperoxide form of Lanthr was observed in solution upon white light irradiation, the same reaction does not occur when Lanthr is part of the metalla-assemblies.

scholarly journals Synthesis and Optoelectronic Properties of Iptycene–Naphthazarin Dyes

Synlett ◽  
2018 ◽  
Vol 30 (01) ◽  
pp. 54-58 ◽  
Author(s):  
Timothy Swager ◽  
Cagatay Dengiz ◽  
You-Chi Wu
Keyword(s):  
Single Crystal ◽  
Electronic Properties ◽  
Diels Alder ◽  
Optoelectronic Properties ◽  
Synthesis And Characterization ◽  
Nmr Analysis ◽  
X Ray ◽  
Vis Spectroscopy

We report the synthesis and characterization of iptycene–naphthazarin dyes by using a sequential Diels–Alder approach. The tautomerization of naphthazarin was used as the key step in the synthesis, with structures confirmed by single-crystal X-ray and NMR analysis. The systematic trends in electronic properties were investigated by UV/Vis spectroscopy. BF2 complexes of the dyes were prepared by reaction with BF3·OEt2 in CH2Cl2.

scholarly journals CAAC Boranes. Synthesis and characterization of cyclic (alkyl) (amino) carbene borane complexes from BF3 and BH3

2010 ◽  
Vol 6 ◽  
pp. 709-712 ◽  
Author(s):  
Julien Monot ◽  
Louis Fensterbank ◽  
Max Malacria ◽  
Emmanuel Lacôte ◽  
Steven J Geib ◽  
...  
Keyword(s):  
Silica Gel ◽  
Synthesis And Characterization ◽  
Gel Chromatography ◽  
Nmr Analysis ◽  
X Ray ◽  
X Ray Crystallography ◽  
In Situ Formation ◽  
Silica Gel Chromatography

In situ formation of two cyclic (alkyl) (amino) carbenes (CAACs) followed by addition of BF3•Et2O provided the first two examples of CAAC–BF3 complexes: 1-(2,6-diisopropylphenyl)-3,5,5-trimethyl-3-phenylpyrrolidin-2-ylidene trifluoroborane, and 2-(2,6-diisopropylphenyl)-3,3-dimethyl-2-azaspiro[4.5]decan-1-ylidene trifluoroborane. These CAAC–BF3 complexes are robust compounds that are stable to ambient laboratory conditions and silica gel chromatography. They were characterized by spectroscopy and X-ray crystallography. In contrast, a CAAC complex with borane (BH3) was readily formed in situ according to 1H and 11B NMR analysis, but did not survive the workup conditions. These results set the stage for further studies of the chemistry of CAAC boranes.

Synthesis and Characterization of a New Infinite 1D Polyoxomolybdate Polymer Further Connected via Cu(I) Nicotinate Subunits

2011 ◽  
Vol 66 (4) ◽  
pp. 351-s357
Author(s):  
Fabienne Gschwind ◽  
Martin Jansen
Keyword(s):  
Single Crystals ◽  
Polymer Chain ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
3D Network

Single crystals of Cu(C6H4NO2)(C6H5NO2)(H2O)2[Mo2O6]n were grown hydrothermally and characterized by X-ray diffraction and elemental analysis. This compound shows a new 1 ∞{Mo2O8}4− infinite polymer chain, which is connected via copper(I) nicotinate subunits, forming an overall 3D network

scholarly journals Darstellung und Charakterisierung der μ3-Oxo-Cluster [Cp3Mo3(CO)4µ-Cl)(µ3-O)] und [Cp3Mo3(µ-CO)3(CO)3(µ3-O)]+ / Synthesis and Characterization of the µ3-Oxo Clusters [Cp3Mo3(CO)4μ-Cl)(μ3-O)] and [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+

1990 ◽  
Vol 45 (4) ◽  
pp. 508-514 ◽  
Author(s):  
B. Nuber ◽  
W. Schatz ◽  
M. L. Ziegler
Keyword(s):  
Structure Analysis ◽  
Elemental Analysis ◽  
Spectroscopic Data ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

[CpMo(CO)3]2 (1) (Cp = cyclopentadienyl) reacts with InCl3 in diglyme to yield the oxo-cluster [Cp3Mo3(CO)4(μ-Cl)(μ3-O)] (2) and the cationic oxo-cluster [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+ as the salt [Cp3Mo3(μ-CO)3(CO)3(μ3-O)][CpMo(CO)3InCl3] (3). The compounds were characterized by elemental analysis, spectroscopic data and X-ray structure analysis. Compound 2 crystallizes in the orthorhombic space group P212121 with a = 1006.0(3), b = 1244.6(4) and c = 1600.8(5) pm, V = 2004.3 x 106 pm3, Z = 4. Compound 3 crystallizes in the monoclinic space group P 21/m with a = 874.4(8), b = 1407(1) and c = 1500(1) pm, β = 92.95(6) , V = 1843 × 106 pm3, Z = 2.

Synthesis and Characterization of a Cubic Iron Hydroxy Boracite

2011 ◽  
Vol 66 (2) ◽  
pp. 107-114 ◽  
Author(s):  
Stephanie C. Neumair ◽  
Johanna S. Knyrim ◽  
Oliver Oeckler ◽  
Reinhard Kaindl ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
High Temperature ◽  
Single Crystals ◽  
Room Temperature ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Pressure High Temperature

The cubic iron hydroxy boracite Fe3B7O13OH・1.5H2O was synthesized from Fe2O3 and B2O3 under high-pressure/high-temperature conditions of 3 GPa and 960 °C in a modified Walker-type multianvil apparatus. The crystal structure was determined at room temperature by X-ray diffraction on single crystals. It crystallizes in the cubic space group F4̄3c (Z = 8) with the parameters a = 1222.4(2) pm, V = 1.826(4) nm3, R1 = 0.0362, and wR2 = 0.0726 (all data). The B-O network is similar to that of other cubic boracites.

A Triple Newman-Kwart Rearrangement at a Fully Substituted Benzene Ring

2009 ◽  
Vol 64 (11-12) ◽  
pp. 1633-1638 ◽  
Author(s):  
Hubert Theil ◽  
Roland Fröhlich ◽  
Thorsten Glaser
Keyword(s):  
Single Crystal ◽  
Benzene Ring ◽  
Structure Analysis ◽  
Synthesis And Characterization ◽  
X Ray ◽  
Benzene Rings

The Newman-Kwart rearrangement of O-thiocarbamates to S-thiocarbamates is a versatile method for the conversion of phenols into thiophenols. The triple rearrangement of the O-trithiocarbamate 2,4,6-triacetyl-1,3,5-tri-(dimethylthiocarbamoyloxy)benzene (2) to the S-trithiocarbamate 2,4,6- triacetyl-1,3,5-tri-(dimethylthiocarbamoylthio)benzene (3) is performed, which is unprecendented for fully substituted benzene rings. The synthesis and characterization of the O-trithiocarbamate 2 and the S-trithiocarbamate 3 including the single-crystal X-ray structure analysis of compound 3 are presented

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