scholarly journals Crystal Structure of Burgess Inner Salts and their Hydrolyzed Ammonium Sulfaminates

2019 ◽  
Vol 72 (11) ◽  
pp. 867 ◽  
Author(s):  
Anthony J. Arduengo III ◽  
Yosuke Uchiyama ◽  
David A. Dixon ◽  
Monica Vasiliu
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crystal Structures ◽  
Ethyl Ester ◽  
Crystallographic Analysis ◽  
Water Soluble ◽  
X Ray ◽  
Dative Bond ◽  
Solid State Structures

The solid-state structures of the Burgess reagent, and its analogous ethyl ester reveal structures indicative of triethylamine solvated sulfonyl imides rather than the more commonly depicted triethylammonium sulfonyl amidate. The existence of a reversibly formed hydrate of Burgess reagent is not supported by present studies, but rather a hydrosylate that does not revert to the Burgess reagent with gentle warming under vacuum was isolated and characterised. Structures of the hydrosylates from both the methyl- and ethyl-amidate esters were determined from X-ray crystallographic analysis and are reported. The crystal structures of the Burgess inner salts exhibit geometries at the sulfur atoms that are intermediate between a planar O2S=NCO2R unit and tetrahedral 4-coordinate sulfur centres that would be expected from a strong single (dative) bond between the triethylamine nitrogen and sulfur. The hydrolysed ammonium sulfaminates are water soluble intermolecular salts composed of triethylammonium ions, Et3NH+, and N-(alkoxycarbonyl)sulfaminate, O(−)SO2NHCO2R {R=CH3 or C2H5}.

Mono- and difunctional furan-based 1,2,3,5-dithiadiazolyl radicals; preparation and solid state structures of 2,5-[(S2N2C)OC4H2(CN2S2)] and 2,5-[(S2N2C)OC4H2(CN)]

1992 ◽  
Vol 70 (3) ◽  
pp. 919-925 ◽  
Author(s):  
A. Wallace Cordes ◽  
Charles M. Chamchoumis ◽  
Robin G. Hicks ◽  
Richard T. Oakley ◽  
Kelly M. Young ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
The Mean ◽  
Solid State Structures ◽  
Solid State Characterization

The preparation and solid state characterization of the bifunctional radical furan-2,5-bis(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN2S2)] and the related monofunctional radical 2-cyanofuran-5-(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN)] are described. The crystal structure of 2,5-[(S2N2C)OC4H2(CN2S2)] is orthorhombic, space group Pna21, and consists of interleaved arrays of dimers, for which the mean interannular [Formula: see text] contact is 3.137 Å. The crystal structure of the monofunctional radical 2,5-[(S2N2C)OC4H2(CN)] is monoclinic, space group P21/n, and consists of a ribbon-like network of dimers (mean interannular [Formula: see text] interconnected by close head-to-tail [Formula: see text] contacts. The dimer units form stacks parallel to z, with a mean interdimer [Formula: see text] separation of 3.956 Å. The similarities and differences between these two crystal structures and those of related benzene-substituted systems are discussed. Keywords: dithiadiazolyl radicals, furan-based diradicals, cyanofuran-based radicals, radical dimers, crystal structures.

scholarly journals Substituent Effects in 3,3’ Bipyrazole Derivatives. X-ray Crystal Structures, Molecular Properties and DFT Analysis

2021 ◽  
Vol 68 (3) ◽  
pp. 718-727
Author(s):  
Ibrahim Bouabdallah ◽  
Tarik Harit ◽  
Mahmoud Rahal ◽  
Fouad Malek ◽  
Monique Tillard ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Density Functional Theory ◽  
Solid State ◽  
Dft Calculations ◽  
Single Crystal ◽  
Crystal Structures ◽  
Density Functional ◽  
Substituent Effects ◽  
Functional Theory ◽  
X Ray

The single crystal X-ray structure of new 1,1’-bis(2-nitrophenyl)-5,5’-diisopropyl-3,3’-bipyrazole, 1, is triclinic P I–, a = 7.7113(8), b = 12.3926(14), c = 12.9886(12) Å, α = 92.008(8), β = 102.251(8), γ = 99.655(9)°. The structural arrangement is compared to that of 5,5’-diisopropyl-3,3’-bipyrazole, 5, whose single crystal structure is found tetragonal I41/a, a = b = 11.684(1), c = 19.158(1) Å. The comparison is also extended to the structures previously determined for 1,1’-bis(2-nitrophenyl)-5,5’-propyl-3,3’-bipyrazole, 2, 1,1’-bis(4-nitrophenyl)-5,5’-diisopropyl-3,3’-bipyrazole, 3, and 1,1’-bis(benzyl)-5,5’-diisopropyl-3,3’-bipyrazole, 4. Density Functional Theory (DFT) calculations are used to investigate the molecular geometries and to determine the global reactivity parameters. The geometry of isolated molecules and the molecular arrangements in the solid state are analyzed according to the nature of the groups connected to the bipyrazole core.

Chemistry and crystal structures of tetrabenzoylethylene, its photolysis product and tetraacetylethylene

1978 ◽  
Vol 31 (6) ◽  
pp. 1265 ◽  
Author(s):  
JR Cannon ◽  
VA Patrick ◽  
CL Raston ◽  
AH White
Keyword(s):  
Solid State ◽  
Crystal Structures ◽  
Molecular Conformation ◽  
Crystallographic Analysis ◽  
Stable Form ◽  
Photolysis Product ◽  
Molecular Conformations ◽  
X Ray ◽  
The Difference ◽  
The Stability

X-ray crystallographic analysis has revealed that the light-sensitive form (A) and the light-stable form (A') of tetrabenzoylethylene are not valence tautomers but are two crystalline modifications of the same substance. The difference in the stability of these forms to light appears to be a consequence of their different molecular conformations and packing in the solid state. The molecular conformation of the A form is represented by (8) and that of the A' form by (9). The related tetraacetylethylene has the conformation (10) in the solid state. X-ray crystallographic analysis has also revealed that the photolysis product (B) of tetrabenzoylethylene is 4-phenoxy-3,4,6-triphenyl-1H,4H-furo[3,4-c]-furan-1-one (11). ��� The crystal structures of (8), (9), (10) and (11) were determined by X-ray diffraction: diffractometer data at 295 K were refined by least-squares techniques to residuals of 0.064 (2161 'observed' reflections) for (8), 0.057 (1310) for (9), 0.049 (1295) for (10) and 0.061 (1639) for (11). Crystals of (8) are monoclinic, P21/n, a 8.775(5), b 17.352(9), c 30.985(8)Ǻ, β 93.01(3)°, Z 8. Crystals of (9) which contain carbon disulfide are monoclinic, A2/a, a 21.21(2), b 6.181(4), c 20.35(2) Ǻ, β 102.77(7)°, Z 4. Crystals of (10) are monoclinic, P21/n, a 7.540(2), b 4.392(2), c 14.770(4) Ǻ, β 96.29(2)°, Z 2. Crystals of (11) are monoclinic, P1/n, a 14.820(4), b 15.000(3), c 10.819(4)Ǻ, β 106.02(2)°, Z 4.

scholarly journals Synthese von Stickstoff- und Chlor-verbrückten Indiumorganylen. Die Kristallstrukturen von [Mes(Cl)InN(SiMe3)2]2 und {i-Pr2In[N(H)t-Bu]2In(Cl)i-Pr} / Synthesis of Nitrogen- and Chloro-Bridged Organoindium Compounds. The Crystal Structures of [Mes(Cl)InN(SiMe3)2]2 and {i-Pr2In[N(H)t-Bu]2In(Cl)i-Pr}

1991 ◽  
Vol 46 (6) ◽  
pp. 753-761 ◽  
Author(s):  
Bernhard Neumüller
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crystal Structures ◽  
Alkyl Aryl ◽  
X Ray ◽  
Sterically Hindered

[(PhCH2)2InN(H)t-Bu]2 (3) and [PhCH2(Cl)InN(SiMe3)2]2 (4) have been prepared by the reaction of (PhCH2)2InCl with LiN(H)t-Bu and of PhCH2InCl2 with NaN(SiMe3)2, respectively. 3 could be isolated in two isomers, while 4 forms only one chloro-bridged isomer in solution and in the solid state. The possibility of a chloro-bridged alkyl(aryl)chloroindium amide is also realized in [Mes(Cl)InN(SiMe3)2]2 (2), as shown by X-ray analysis. The reaction of a 1:1-mixture of i-Pr2InCl/i-PrInCl2 with LiN(H)t-Bu leads to all three possible compounds: [i-Pr(Cl)InN(H)t-Bu]2 (1), {i-Pr2In[N(H)t-Bu]2In(Cl)i-Pr} (5), and [i-Pr2InN(H)t-Bu]2 (6). Two isomers of the new compound 5 are detectable in solution. The crystal structure has been determined for the less sterically hindered isomer 5a, which forms hydrogen-bridged (Cl-H-N-bridge) infinite chains along the c-axis.

meso–meso Directly-linked trimeric and pentameric electron-deficient porphyrin–hexaphyrin hybrid arrays

2016 ◽  
Vol 20 (01n04) ◽  
pp. 245-253 ◽  
Author(s):  
Hirotaka Mori ◽  
Atsuhiro Osuka
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solid State Structures

meso–meso Directly-linked trimeric and pentameric porphyrin–hexaphyrin hybrid arrays 5 and 6 comprising of electron-deficient porphyrin units were prepared by cross-condensation of monomeric and dimeric electron-deficient meso-formyl porphyrins with a tripyrrane. The solid-state structures of 5 and 6 have been determined by single crystal X-ray diffraction analysis. The latter is the largest crystal structure of meso–meso linked multiporphyrinic array analogues reported to date.

scholarly journals Synthesis and Solid-state Structures of 1,3- and 1,4-Bis(diethylgallyl) benzene

2009 ◽  
Vol 64 (11-12) ◽  
pp. 1375-1380
Author(s):  
Joseph Izundu ◽  
Peter Jutzi ◽  
Beate Neumann ◽  
Henning Sielemann ◽  
Hans-Georg Stammler
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structure Analysis ◽  
Crystal Structure Analysis ◽  
Structural Studies ◽  
X Ray ◽  
Coordination Behavior ◽  
Redistribution Reactions ◽  
Solid State Structures

The compounds 1,3-bis(diethylgallyl)benzene (3) and 1,4- bis(diethylgallyl)benzene (6) were prepared by reaction of the corresponding chloromercuriobenzenes with an excess of triethylgallium by applying pressure and higher temperatures. These compounds very easily undergo redistribution reactions in solution and in the solid state. Extremely air-sensitive crystals suitable for an X-ray crystal structure analysis were obtained from triethylgallium as solvent. The structural studies revealed the presence of tetra-coordinated carbon and gallium atoms in symmetric aryl-diethylgallyl bridging units. The coordination behavior of 3 and 6 in the solid state is quite different from that of the corresponding methyl-substituted compounds

Heterocyclic Tautomerism. IV. The Solution and Crystal Structures of 1-Aryl-3-phenyl-1,2,4-triazol-5-ones

1988 ◽  
Vol 41 (4) ◽  
pp. 419 ◽  
Author(s):  
AD Rae ◽  
CG Ramsay ◽  
PJ Steel
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Solid State ◽  
Crystal Structures ◽  
Complex Network ◽  
Water Molecules ◽  
X Ray ◽  
Structure Determinations ◽  
Hydrogen Bonded

The title compounds are shown to exist in solution and in the solid state as 4H-tautomers. X-Ray crystal structure determinations show that 1,3-diphenyl-1,2,4-triazol-5-one exists as a dimeric pair of strongly hydrogen-bonded molecules and that 3-phenyl-1-(2-pyridyl)-1,2,4- triazol-5-one exists as the 4H-tautomer stabilized by a complex network of hydrogen bonding to water molecules.

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