Neue Cyclophosphazene mit Metallen der III. Hauptgruppe als Ringbausteine / New Cyclophosphazenes with Metals of Main Group III as Building Blocks

1994 ◽  
Vol 49 (1) ◽  
pp. 43-49 ◽  
Author(s):  
Reinhard Hasselbring ◽  
Herbert W. Roesky ◽  
Andreas Heine ◽  
Dietmar Stalke ◽  
George M. Sheldrick
Keyword(s):  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Building Blocks ◽  
Main Group ◽  
Ring Formation ◽  
Lewis Acidity ◽  
X Ray ◽  
Group Iii ◽  
Space Groups ◽  
Ring Compounds

Abstract Acylic silylated phosphazenes of the type HN(PR2NSiMe3)2 (1) react quantitatively with molecules MMe3 (M = Al, Ga, In) under ring formation and CH4 evolution. The ring compounds N(PPh2NSiMe3)2AlMe2 (2 a) and N(PPh2NSiMe3)2InMe2 (4 a) have been investiga­ ted by X-ray structure determination. 2a and 4a crystallize in the space groups P 1̄ and P 31, respectively; they show different conformations regarding the cyclohexane framework. NMR spectroscopy of the nuclei in the chelating phosphazene ligand indicates decreasing Lewis acidity of the metal containing fragments in the series AlMe2 ≥ GaMe2 > InMe2.

scholarly journals 2-(3,5-Dimethyl-1H-pyrazol-1-yl)thiazolo[4,5-b]pyridine

Molbank ◽  
10.3390/m1077 ◽  
2019 ◽  
Vol 2019 (3) ◽  
pp. M1077
Author(s):  
Lan ◽  
Zheng ◽  
Wang
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
1H Nmr ◽  
Structure Determination ◽  
1H Nmr Spectroscopy ◽  
Pyrazole Ring ◽  
Hydrogen Atoms ◽  
X Ray ◽  
X Ray Crystallography

The compound 2-(3,5-dimethyl-1H-pyrazol-1-yl)thiazolo[4,5-b]pyridine (1) was synthesized with a yield of 71% by the reaction of 1-(thiazolo[4,5-b]pyridine-2-yl)hydrazine and acetylacetone. The structure was characterized by a single-crystal X-ray structure determination as well as 1H and 13C{1H} NMR spectroscopy. X-ray crystallography on 1 confirms the molecule consists of a pyridine–thiazole moiety and the pyrazole ring, and all non-hydrogen atoms are planar.

scholarly journals Synthesis and Single Crystal X-Ray Structure of Bis[4-oxo-3- (2-ethoxycarbonylphenyl)-3,4-dihydroquinazolin-2-yl]disulfide

2009 ◽  
Vol 64 (9) ◽  
pp. 1065-1069 ◽  
Author(s):  
Mehdi Rimaz ◽  
Jabbar Khalafy ◽  
Khadijeh Tavana ◽  
Katarzyna Ślepokura ◽  
Tadeusz Lis ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Structure Determination ◽  
Room Temperature ◽  
Sodium Ethoxide ◽  
Reaction Conditions ◽  
X Ray ◽  
Ethyl Nitroacetate ◽  
C Nmr

Diethyl 2,2´-thiocarbonyl-bis(azanediyl)dibenzoate was synthesized from the reaction of ethyl anthranilate with thiophosgene. Its treatment with sodium ethoxide in ethanol at room temperature gave ethyl 2-(4-oxo-2-thioxo-1,2-dihydroquinazolin-3(4H)-yl) benzoate, whereas in the presence of ethyl nitroacetate and under the same reaction conditions, the corresponding bis(quinazolin)disulfide was formed. Its structure was confirmed by IR, 1H and 13C NMR spectroscopy elemental analysis and single crystal X-ray structure determination.

Structure determination of a partially ordered layered silicate material with an NMR crystallography approach

2017 ◽  
Vol 73 (3) ◽  
pp. 184-190 ◽  
Author(s):  
Darren Henry Brouwer ◽  
Sylvian Cadars ◽  
Kathryn Hotke ◽  
Jared Van Huizen ◽  
Nicholas Van Huizen
Keyword(s):  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Three Dimensional ◽  
Layered Silicate ◽  
Silicate Layer ◽  
Silicate Material ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Crystallography

Structure determination of layered materials can present challenges for conventional diffraction methods due to the fact that such materials often lack full three-dimensional periodicity since adjacent layers may not stack in an orderly and regular fashion. In such cases, NMR crystallography strategies involving a combination of solid-state NMR spectroscopy, powder X-ray diffraction, and computational chemistry methods can often reveal structural details that cannot be acquired from diffraction alone. We present here the structure determination of a surfactant-templated layered silicate material that lacks full three-dimensional crystallinity using such an NMR crystallography approach. Through a combination of powder X-ray diffraction and advanced 29Si solid-state NMR spectroscopy, it is revealed that the structure of the silicate layer of this layered silicate material templated with cetyltrimethylammonium surfactant cations is isostructural with the silicate layer of a previously reported material referred to as ilerite, octosilicate, or RUB-18. High-field 1H NMR spectroscopy reveals differences between the materials in terms of the ordering of silanol groups on the surfaces of the layers, as well as the contents of the inter-layer space.

scholarly journals Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids

2013 ◽  
Vol 117 (23) ◽  
pp. 12258-12265 ◽  
Author(s):  
Dmytro V. Dudenko ◽  
P. Andrew Williams ◽  
Colan E. Hughes ◽  
Oleg N. Antzutkin ◽  
Sitaram P. Velaga ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Solid State Nmr ◽  
Molecular Solids ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solid State Nmr Spectroscopy

Lewis-Base Adducts of Main Group 1 Metal Compounds. V. Diaquabis(quinoline)lithium(I) Bromide Bis(quinoline)

1988 ◽  
Vol 41 (3) ◽  
pp. 409 ◽  
Author(s):  
CL Raston ◽  
BW Skelton ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
Lithium Bromide ◽  
Main Group ◽  
Lewis Base ◽  
Metal Compounds ◽  
X Ray ◽  
Group 1

The title compound, an artefact of recrystallization of lithium bromide from improperly dried quinoline, has been characterized by a single- crystal X-ray structure determination. Crystals are triclinic, Pī , a 16.608(9), b 12.27(1), c 7.962(8)Ǻ, α 101.98(8),β 91.79(7),γ 92.27(6), Z 2; R was 0.058 for 2404 'observed' reflections. The cation is the first to be structurally defined for a [Li(OH2)2 (N-base)2]+ system; Li-O are 1.92(2), 1.93(2)Ǻ and Li-N 2.12(2), 2.14(2)Ǻ.

Computational challenges for macromolecular structure determination by X-ray crystallography and solution NMRspectroscopy

1993 ◽  
Vol 26 (1) ◽  
pp. 49-125 ◽  
Author(s):  
Axel T. Brünger ◽  
Michael Nilges
Keyword(s):  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Solution Nmr ◽  
Macromolecular Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
The Past ◽  
Solution Nmr Spectroscopy

Macromolecular structure determination by X-ray crystallography and solution NMR spectroscopy has experienced unprecedented growth during the past decade.

scholarly journals Solutions of Gallium Trichloride in Ethers: A 71Ga NMR Study and the X-Ray Structure of GaCl3 · Monoglyme

1990 ◽  
Vol 45 (7) ◽  
pp. 979-984 ◽  
Author(s):  
Stefan Böck ◽  
Heinrich Nöth ◽  
Astrid Wietelmann
Keyword(s):  
Nmr Spectroscopy ◽  
Structure Determination ◽  
X Ray ◽  
Predominant Species ◽  
Nmr Study ◽  
Gallium Trichloride

Solutions of GaCl3 in various ethers have been studied by 71Ga NMR spectroscopy. σ71Ga data indicate that the predominant species in diethylether and tetrahydrofuran solutions are GaCl3 · O(C2H5)2 and GaCl3. 2OC4H8, respectively. However, in monoglyme solution dissociation occurs and the product crystallizing from the solution is [cis-GaCl2(monoglyme)2]GaCl4 as demonstrated by an X-ray structure determination of the solvate GaCl3 · monoglyme.

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