scholarly journals Isolation and structure determination of a tetrameric sulfonyl dilithio methandiide in solution based on crystal structure analysis and 6Li/13C NMR spectroscopic data

2020 ◽  
Vol 16 ◽  
pp. 2057-2063
Author(s):  
Jürgen Vollhardt ◽  
Hans Jörg Lindner ◽  
Hans-Joachim Gais
Keyword(s):  
Crystal Structure ◽  
Characteristic Feature ◽  
Structure Analysis ◽  
13C Nmr ◽  
Structure Determination ◽  
Low Temperatures ◽  
Spectroscopic Data ◽  
Crystal Structure Analysis ◽  
Fast Exchange

Dilithio sulfonyl methandiides are a synthetically and structurally highly interesting group of functionalized geminal dianions. Although very desirable, knowledge of the structure of dilithio methandiides in solution was lacking up to now. Herein, we describe the isolation and determination of the structure of tetrameric dilithio (trimethylsilyl)(phenylsulfonyl) methandiide in solution and in the crystal. The elucidation of the structure of the tetramer is based on crystal structure analysis and 13C/6Li NMR spectroscopic data. A characteristic feature of the structure of the tetramer is the C 2 symmetric C–Li chain, composed of four doubly Li-coordinated dianionic carbon and five Li atoms. Three Li atoms are devoid of a contact to a dianionic C atom. The tetramer, the dianionic C atoms of which undergo fast exchange, is in THF solution in fast equilibrium with a further aggregate, which is stable only at low temperatures.

The Use of Optical Transforms in Crystal-Structure Analysis

1960 ◽  
Vol 4 ◽  
pp. 1-18
Author(s):  
Arnold Hargreaves
Keyword(s):  
Crystal Structure ◽  
Diffraction Pattern ◽  
Structure Analysis ◽  
Structure Determination ◽  
Crystal Structure Analysis ◽  
Fraunhofer Diffraction ◽  
X Ray ◽  
Simple Instrument ◽  
Optical Transform

AbstractOptical transforms are of particular value In the earlier stages of crystal-structure determination; they enable trial structures to be tested rapidly and may indicate the nature of changes which will improve a postulated structure. The optical transforms are produced in a simple instrument called an optical diffractometer. The projected positions of the atoms in a postulated structure are represented by a set of holes punched in a mask, and the diffractometer produces the Fraunhofer diffraction pattern of the mask. The distribution of intensity in the optical transform is comparable, when sampled at suitable Intervals, with the distribution of intensity among the observed intensities in a particular zone of X-ray reflections. The use of optical transforms in the determination of crystal structures and in the study of imperfect structures will be illustrated by examples.

Synthese und Kristallstrukturanalyse von Undecacarbonyl- (μ-trifluormethylisocyanid)trieisen, Fe3(μ-CNCF3)(CO)11 / Synthesis and Crystal Structure Determination of Undecacarbonyl(μ-trifluoromethylisocyanide)triiron, Fe3(μ-CNCF3)(CO)11

1984 ◽  
Vol 39 (6) ◽  
pp. 721-726 ◽  
Author(s):  
Irene Brüdgam ◽  
Hans Hartl ◽  
Dieter Lentz
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structure Analysis ◽  
Structure Determination ◽  
Crystal Structure Analysis ◽  
Crystal Structure Determination ◽  
Synthesis And Crystal Structure ◽  
Infrared Data ◽  
C Nmr

AbstractThe unstable trifluorom ethylisocyanide can be stabilized on the Fe3(CO)11 framework. Infrared data suggest that the isocyanide ligand occupies bridging positions in the solid state and in solution. This fact has been confirmed by the crystal structure analysis and by 13C NMR measurements.

scholarly journals Preparative-scale HPLC Resolution of Metallacyclic η3-Allyltricarbonyliron Complexes and Determination of the Absolute Configuration by X-Ray Crystal Structure Analysis

1999 ◽  
Vol 23 (9) ◽  
pp. 578-579
Author(s):  
Rainer Schobert ◽  
Hermann Pfab ◽  
Jutta Böhmer ◽  
Frank Hampel ◽  
Andreas Werner
Keyword(s):  
Crystal Structure ◽  
Silica Gel ◽  
Structure Analysis ◽  
Absolute Configuration ◽  
Crystal Structure Analysis ◽  
Preparative Scale ◽  
X Ray ◽  
The Absolute

Racemates of (η3-allyl)tricarbonyliron lactone complex Fe(CO)3{η1:η3-C(O)XCH2CHCMeCH2} 1a (X = O) and (η3-allyl)tricarbonyliron lactam complex 2a (X = NMe) are resolved on a preparative scale by HPLC on cellulose tris(3,5-dimethylphenyl)carbamate/silica gel RP-8 and the absolute configuration of (-)-2a is determined by X-ray crystal structure analysis.

scholarly journals (2S,3S,4R,4a'R,5R,5a'R,11a'R,12′S,12a'R)-5-(Acetoxymethyl)-2′,2′,10′,10′-tetramethyloctahydro-3H,8′H-spiro[furan-2,7′-[1,3]dioxino[4′,5′:5,6]pyrano[3,2-d][1,3,6]trioxocine]-3,4,12′-triyl triacetate

IUCrData ◽  
2019 ◽  
Vol 4 (7) ◽  
Author(s):  
H. E. Bollard ◽  
M. G. Banwell ◽  
J. S. Ward
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Absolute Configuration ◽  
Title Compound ◽  
Resonant Scattering ◽  
Crystal Structure Analysis ◽  
Compound C ◽  
Synthetic Derivative

While the crystal structure analysis of the title compound, C26H38O15, a synthetic derivative of sucrose, was originally reported 40 years ago [Drew et al. (1979). Carbohydr. Res. 71, 35–42], the present work has allowed for the determination of its absolute configuration through the application of resonant scattering techniques.

The Structure of the Novel Lichen Xanthone Thiomelin and Its Cogenors

1987 ◽  
Vol 40 (7) ◽  
pp. 1169 ◽  
Author(s):  
JA Elix ◽  
KL Gaul ◽  
M Sterns ◽  
MW Binsamsudin
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Ring Opening ◽  
Spectroscopic Data ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Lichen Metabolite

The structure determination of thiomelin (2,4-dichloro-1,8-dihydroxy-5-methoxy-6-methyl-9H-xanthen-9-one) (3), an unusual lichen metabolite probably derived biosynthetically by oxidative ring opening of a precursor anthraquinone, is reported. The crystal structure of thiomelin diacetate (4) was determined by X-ray diffraction, while that of the cogenors 8-O-methylthiomelin (5), 4-dechlorothiomelin (7), 4-dechloro-8- O- methylthiomelin (9), 2-dechloro-8- O- methylthiomelin (10) and 2,4-dichloro-l-hydroxy-7-methoxy-6,8-dimethyl-9H-xanthen-9-one (12) were deduced from spectroscopic data.

Preparation and Crystal Structure Determination of [(C2Η5)4N]2Hg3Cl8

1995 ◽  
Vol 50 (1) ◽  
pp. 66-70 ◽  
Author(s):  
Inge Pabst ◽  
Peter Sondergeld ◽  
Mirjam Czjzek ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Analysis ◽  
Structure Determination ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Coordination Type ◽  
X Ray

The title compound has been prepared in two different ways: First, by boiling single crystals of [(C2H5)4N]HgCl3 in a mixture of n-hexane/n-octane [4:1] at T = 350 K, and second, in a synthesis from stoichiometric quantities of the components. X-ray structure analysis gave the stoichiometry [(C2H5)4N]2Hg3Cl8, monoclinic, space group P21, a = 7.538(3), b = 19.909(6), c = 10.274(3) Å, β = 95.13(1)°, V = 1535.7(9) A3, Z = 2. The basic [Hg3Cl8]2--units form broken zig-zag chains along [100]. The Hg–Cl distances within the [Hg3Cl8]2- clusters range from 2.315(3) to 2.755(4) Å. This is a new coordination type for halomercurates.

X-Ray crystal structure analysis and determination of azo-enamine and hydrazone-imine tautomers of two hetarylazo indole dyes

2007 ◽  
Vol 123 (6) ◽  
pp. 358-364 ◽  
Author(s):  
Süheyla Özbey ◽  
Arzu Karayel ◽  
Gülten Kavak ◽  
Zeynel Seferoğlu ◽  
Nermin Ertan
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Crystal Structure Analysis ◽  
X Ray
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