β-octabromo-meso-tris(pentafluorophenyl)corrole: reductive demetalation-based synthesis of a heretofore inaccessible, perhalogenated free-base corrole

2010 ◽  
Vol 14 (06) ◽  
pp. 509-512 ◽  
Author(s):  
Can Capar ◽  
Lars-Kristian Hansen ◽  
Jeanet Conradie ◽  
Abhik Ghosh
Keyword(s):  
Copper Complex ◽  
Free Ligand ◽  
Crystallographic Analysis ◽  
The Other ◽  
High Yield ◽  
Free Base ◽  
X Ray ◽  
The Mean

Long known in various metal-complexed forms, β-octabromo-meso-tris(pentafluorophenyl)corrole, H3[Br8TPFPC ], has not been available as a free ligand until now. It can be prepared in high yield (86%) via reductive demetalation (conc. H2SO4 , FeCl2 ) of Mn[Br8TPFPC ]. Interestingly, the same conditions did not result in demetalation of the analogous copper complex, which may be contrasted to the behavior of many other copper corroles, which demetalate cleanly. X-ray crystallographic analysis revealed a unique "half-saddled" conformation, wherein two of the pyrrole rings on one side of the direct pyrrole-pyrrole linkage are strongly tilted up and down relative to each other, whereas the other two pyrrole rings are roughly in the mean plane of the macrocycle.

Isoelastic Cementless Total Hip Replacement in Rheumatoid Arthritis. Long-Term Results

1992 ◽  
Vol 2 (2) ◽  
pp. 43-46
Author(s):  
U. Fusco ◽  
R. Capelli ◽  
A. Avai ◽  
M. Gerundini ◽  
L. Colombini ◽  
...  
Keyword(s):  
Rheumatoid Arthritis ◽  
Hip Replacement ◽  
The Other ◽  
Long Term Results ◽  
X Rays ◽  
X Ray ◽  
The Mean ◽  
Cementless Total Hip Replacement

Between 1980 and 1987 we have implanted 46 isoelastic cementless THR in 40 patients affected with rheumatoid arthritis. We have reviewed 38 hips clinically and by X-ray. The mean follow-up was 8,5 years. Harris hip scores ranged from 30.6 preoperatively to 73,4 post-operatively when reviewed. While on the other hand Merle D'Aubigné hip scores ranged from 7,06 pre-operatively to 15,59 post-operatively. All patients have been satisfied, and X-rays showed an improvement for both Charnely and Gruen X-ray score.

scholarly journals Synthesis and Structural Elucidation of the Acetylation Reaction’s Product(s) of the 2(1H)-Quinoxalinones Derived from L-Ascorbic Acid. X-Ray Molecular Structure of 3-(N-acetyl-2-naphthylhydrazono)-2,3-dihydro-2-acetoxyfuro[2,3-b]quinoxaline [1]

1992 ◽  
Vol 47 (6) ◽  
pp. 861-868 ◽  
Author(s):  
Adel Amer ◽  
Douglas M. Ho
Keyword(s):  
Molecular Structure ◽  
Ascorbic Acid ◽  
Acetic Anhydride ◽  
Structural Elucidation ◽  
Ring Closure ◽  
The Other ◽  
High Yield ◽  
X Ray ◽  
Reaction Condition ◽  
Tricyclic Compound

Acetylation reaction’s product(s) of 3-[L-threo-2,3,4-trihydroxy-1-(2-naphthylhydrazono)-butyl]quinoxalin-2(1H)-one (2b) were found to be dependent on the reaction condition. While the tri-O-acetyl (3b) was isolated in high yield from 2b under the action of acetic anhydride/pyridine mixture, compounds 4b and 5b as well as trace of 3b were obtained when 2b was heated in acetic anhydride. On the other hand, 3-[1-(2-naphthylhydrazono)-glyoxal-1-yl]quinoxalin-2(1H)-one (7) underwent ring closure and afforded the condensed tricyclic compound 8 under the action of acetic anhydride/pyridine mixture.

scholarly journals Attempted Synthesis and Unexpected β-Fragmentation of a Hindered β-Keto Nitroxide

2017 ◽  
Vol 70 (10) ◽  
pp. 1106 ◽  
Author(s):  
Chris Edwards ◽  
Peter C. Healy ◽  
W. Ken Busfield ◽  
Ezio Rizzardo ◽  
San H. Thang ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Ring Opening ◽  
Sodium Tungstate ◽  
Crystallographic Analysis ◽  
High Yield ◽  
Fragmentation Mechanism ◽  
Pentanoic Acid ◽  
X Ray ◽  
Ring Opening Reaction

The attempted synthesis of a β-keto imidazolidinone nitroxide by oxidation of the β-hydroxy imidazolidinone precursor with hydrogen peroxide and sodium tungstate led to an unexpected ring-opening reaction to produce 1,4-diazaspiro[4.5]dec-1-en-3-oxo-2-pentanoic acid 1-oxide (13) in high yield. The structure of 13 was confirmed by X-ray crystallographic analysis. A β-fragmentation mechanism is suggested for the oxidative ring-opening reaction.

The direct electrochemical synthesis of thiolato complexes of cobalt and nickel, and the crystal structure of bis(phenylthiolato)bis(1,10-phenanthroline)cobalt(III) perchlorate

1988 ◽  
Vol 66 (9) ◽  
pp. 2151-2156 ◽  
Author(s):  
Raj K. Chadha ◽  
Rajesh Kumar ◽  
Jaime Romero Lopez-Grado ◽  
Dennis G. Tuck
Keyword(s):  
Crystal Structure ◽  
Electrochemical Oxidation ◽  
Electrochemical Synthesis ◽  
Crystallographic Analysis ◽  
High Yield ◽  
X Ray ◽  
Metal Anode ◽  
Aerial Oxidation ◽  
Perchlorate Salt ◽  
Cobalt And Nickel

Cobalt(II) and nickel(II) thiolates, M(SR)2, can be prepared in high yield by the electrochemical oxidation of a metal anode in an acetonitrile or acetone solution of RSH (R = C6H5, o-CH3C6H4, 2-C10H7, 2,3,4,5-C6F4H; not all combinations). When 2,2-bipyridine or 1,10-phenanthroline (=L) is added to the electrolyte phase, the products are the adducts M(SR)2L2. In the case of Co(SC6H5)2(phen)2, aerial oxidation leads to the formation of the cobalt(III) cation [Co(SC6H5)2(phen)2]+, isolated as the perchlorate salt. X-ray crystallographic analysis showed that this cation has a cis-CoS2(N2)2 kernel.

Synthesis, spectroscopic and structural analysis of a melamine copper complex

2014 ◽  
Vol 70 (a1) ◽  
pp. C1239-C1239
Author(s):  
Amani Direm ◽  
Noureddine Dadda ◽  
Wahiba Falek ◽  
Zina Boutobba ◽  
Nourredine Benali-Cherif
Keyword(s):  
Structural Analysis ◽  
Copper Complex ◽  
Structural Investigation ◽  
Three Dimensional ◽  
Building Blocks ◽  
The Other ◽  
X Ray Diffraction ◽  
X Ray ◽  
Supramolecular Architectures ◽  
Carboxylic Anions

Owing to its multiple sites acting as H-bonds' donors, melamine and its derivatives are considered as excellent building blocks for the construction of various crystalline supramolecular architectures based on phosphate, sulfate, chloride and carboxylic anions [1-10] on one hand and chlorometallate anions on the other hand [11-13]. In our contribution, we will discuss the synthesis, FTIR spectra and the structural investigation using the single crystal X-ray diffraction of (H2Melamine) [CuCl5]Cl, (I). The structural analysis of (I) revealed that it consists of alternating negative and positive layers running through the a-axis direction. The negative layers are built up of alternatively CuCl53- and discrete non-coordination Cl- anions, whereas the positive sheets are formed of [H2melamine2+]2 Hydrogen-bonded dimers. The N-H...N and N-H...Cl interactions are assembled to build three-dimensional H-bond patterns which insure the cohesion within the lattice (Fig. 01). A previous work showed that (I) exhibits antiferromagnetic properties [14]

Synthesis and X-ray crystallographic analysis of free base and hexafluorophosphate salts of 3,4-dihydroisoquinolines from the Bischler–Napieralski reaction

2021 ◽  
Author(s):  
Carlos E. Puerto Galvis ◽  
Cristian C. Granados ◽  
Vladimir V. Kouznetsov ◽  
Mario A. Macías
Keyword(s):  
Crystallographic Analysis ◽  
Free Base ◽  
X Ray ◽  
Reaction Potential

Free base and hexafluorophosphate salts of 3,4-dihydroisoquinolines from the Bischler–Napieralski reaction: potential supramolecular modulation. Centrosymmetric/enantiomorphic crystals.

scholarly journals Synthesis of Some Biologically Important 3-Oxacepham Derivatives

1970 ◽  
Vol 5 (1) ◽  
pp. 47-51 ◽  
Author(s):  
Mohammad Rafiqul Islam ◽  
Mohammad Nurnabi ◽  
AM Sarwaruddin Chowdhury ◽  
Mohammad Mehdi Masud
Keyword(s):  
Key Words ◽  
Full Text ◽  
Crystallographic Analysis ◽  
High Yield ◽  
Methyl Group ◽  
X Ray ◽  
Tert Butyl ◽  
Relative Stereochemistry

The 6H-oxathiazines 1a-e having imine moiety underwent [2+2] cycloaddition with phenoxyacetylchloride in the presence of Et3N to give β-lactam derivatives 2a-e in high yield. The X-ray crystallographic analysis revealed the relative stereochemistry that the substituents at C-2 and C-4 were cis configurated. The subtituents at C-6 and C-7 were also cis to each other. However, the 6H-oxathiazines 1f-i containing tert-butyl or methyl group at C-4 did not undergo the cycloaddition. Key words: Azetedinone, β-lactam, oxacepham, cycloaddition, imine, ketene, oxathiazine. Dhaka Univ. J. Pharm. Sci. Vol.5(1-2) 2006 The full text is of this article is available at the Dhaka Univ. J. Pharm. Sci. website

scholarly journals Effect of the Dog positioning on X-Ray Table on Hip Dysplasia Parameter Evaluation

2019 ◽  
Vol 32 (05) ◽  
pp. 376-382 ◽  
Author(s):  
João Martins ◽  
Bruno Colaço ◽  
Sofia Alves-Pimenta ◽  
José M. Gonzalo Orden ◽  
António J. Ferreira ◽  
...  
Keyword(s):  
Hip Dysplasia ◽  
External Rotation ◽  
The Other ◽  
Femoral Rotation ◽  
X Ray ◽  
Parameter Evaluation ◽  
Retrospective Clinical Study ◽  
The Mean ◽  
Study Type ◽  
Norberg Angle

Abstract Objective The aim of this study was to evaluate the effect of pelvic tilting along the long axis and femoral rotation on Norberg angle (NA), subluxation index (SI) and subluxation category (SC) in the standard ventrodorsal hip extended (VDHE) radiographical view on live animals. Study Type This was a retrospective clinical study. Materials and Methods Pairs of VDHE views, one adequately positioned and the other with pelvic tilting or femoral internal or external rotation, were compared for the NA, SI and SC. Results On the malpositioned pelvis set, on the underside the mean ± SD NA was 98.7 ± 6.1°, the SI was 0.27 ± 0.12 and the SC was 2.8 ± 0.8 versus, on the acceptable set, the NA was 99.2 ± 6.4° (p > 0.05), the SI was 0.25 ± 0.12 (p < 0.05) and the SC was 2.3 ± 0.9 (p < 0.05); on the malpositioned upperside, the NA was 102.1 ± 6.4°, the SI was 0.21 ± 0.14 and the SC was 1.7 ± 1.1 versus, on the acceptable positioned set, the NA was 100.8 ± 6.7° (p < 0.05), the SI was 0.24 ± 0.15 (p < 0.05) and the SC was 2.3 ± 1.2 (p < 0.05). Femoral internal or external rotation sets did not show significant differences between malpositioned and acceptable positioned sets (p > 0.05). Conclusions In clinical practice, pelvic tilting along the long axis in VDHE view results in non-favourable hip changes in the NA, SI and SC on the underside and favourable on the upperside, and the internal or external femoral rotation did not affect these variables.

scholarly journals X-ray microanalysis of aldehyde-fixed glycogen contrast-stained by OsVI . FeII and OsVI . RuIV complexes.

1980 ◽  
Vol 28 (11) ◽  
pp. 1242-1250 ◽  
Author(s):  
W C de Bruijn ◽  
J M van Buitenen
Keyword(s):  
Electron Microscope ◽  
Complex Formation ◽  
Rat Liver ◽  
Lipid Droplets ◽  
Liver Glycogen ◽  
The Other ◽  
Glutaraldehyde Fixation ◽  
Fixed Tissue ◽  
X Ray ◽  
The Mean

The composition of the contrast-donating complex of rat liver glycogen, nucleoplasm, erythrocytes, and mitochondria was established by X-ray microanalysis. In these compartments the presence of osmium and iron was shown qualitatively in tissue after glutaraldehyde fixation, treated with OsVIIIO4 plus K4FeII(CN)6 and in similar tissue treated with a combination of K2OsVIO4 plus K4FeII(CN)6. Osmium and ruthenium were detected in these compartments, in aldehyde-fixed tissue treated with mixtures containing K2RuIVL(CN)6 rather than K4FeII(CN)6. The iron detected in the glycogen, nucleoplasm, erythrocytes, and mitochondria of tissue treated with K2RuIV(CN)6 mixtures proved to derive from sources inside the electron microscope, and had to be considered an artifact. Quantitatively, the mean atomic ratios of osmium-to-iron and osmium-to-ruthenium were determined from spectra obtained by point analyses of the same compartments (glycogen, nucleoplasm, mitochondria, lipid droplets, and erythrocytes). After correction of the spectra for the instrumental iron contribution, the osmium-to-iron and osmium-to-ruthenium ratios in the glycogen were about 1:3 for tissue treated with those combinations including K2OsVIO4. In the other compartments, the osmium-to-iron and osmium-to-ruthenium ratios were virtually 1:0. For Os-VIIIO4 in combination with potassium ferrouscyanide however the osmium-to-iron ratio was 1:7 in the glycogen and 1:5 in all other compartments. OsVIIIO4 was combined with potassium ruthenium-cyanide, the osmium-to-ruthenium ratio was 1:2 in the glycogen and 2:1 in the other compartments. These results support our view that the selective glycogen contrast is obtained by complex formation.

Preparation of Magnetic Ionic Liquids Composed of Hybrid-Type Anions

2012 ◽  
Vol 65 (11) ◽  
pp. 1557 ◽  
Author(s):  
Yumiko Takagi ◽  
Yoriko Kusunoki ◽  
Yukihiro Yoshida ◽  
Hirofusa Tanaka ◽  
Gunzi Saito ◽  
...  
Keyword(s):  
Ionic Liquid ◽  
Magnetic Property ◽  
Ionic Liquids ◽  
Crystallographic Analysis ◽  
The Other ◽  
X Ray ◽  
Magnetic Ionic Liquids ◽  
Hybrid Type ◽  
Magnetic Ionic Liquid ◽  
Chloride Hydrate

1-Ethyl-3-methylimidazolium ethylsulfate ([C2mim][EtSO4]) was mixed with iron(III) chloride·6H2O to give a magnetic ionic liquid composed of the hybrid-type anion, [C2mim][FeCl3·EtSO4], which showed a slightly different magnetic property than [C2mim][FeCl4]. On the other hand, reaction of [C2mim][EtSO4] with cobalt(II) chloride hydrate formed [C2mim]2[CoIICl4], the structure of which was characterised by X-ray crystallographic analysis.

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