Selenium coronands. A novel conformational pair

1988 ◽  
Vol 66 (11) ◽  
pp. 2956-2958 ◽  
Author(s):  
B. Mario Pinto ◽  
Blair D. Johnston ◽  
Raymond J. Batchelor ◽  
Frederick W. B. Einstein ◽  
Ian D. Gay
Keyword(s):  
Nmr Spectra ◽  
Crystallographic Analysis ◽  
The Novel ◽  
Torsion Angles ◽  
X Ray ◽  
Structure Formula ◽  
Independent Molecules ◽  
Similar Conformation ◽  
C Nmr

The synthesis and characterization of the novel selenium coronands, 1,3,7,9-tetraselenacyclododecane 1a, 1,3,7,9,13,15-hexaselenacyclooctadecane 2a, the corresponding β-gem-dimethyl derivatives 1b, 2b, and 1,5,9,13-tetraselenacyclohexadecane 3, and 1,5,9,13,17,21-hexaselenacyclotetracosane 4 are described. X-ray crystallographic analysis of 1a reveals three independent molecules that exist in two distinct conformations, one molecule having approximate two-fold symmetry together with two molecules (of similar conformation) each having crystallographic [Formula: see text] symmetry. The conformations are denoted as [3333] or [66]. Whereas one resembles that of cyclododecane and tetrathia-12-crown-4 with respect to torsion angles, the other resembles that of tetraoxa-12-crown-4. The solid state CP-MAS 77Se and 13C nmr spectra are interpreted in light of the crystallographic information. Crystal structure: formula Se4C8H16; fw = 428.05; monoclinic, P21/c; Z = 8; a = 15.823(2) Å, b = 5.534(1) Å, c = 27.962(5) Å, β = 92.26(1)°; V = 2446.6 Å3; T = 200 K; R = 0.027 for 2162 observed data (I ≥ 2.5σ(I)).

Far-red absorbing azodipyrrin dyes — Synthesis, X-ray crystallographic, and spectral characterization of 1,9-diazodipyrrins and their metal complexes

2011 ◽  
Vol 89 (4) ◽  
pp. 481-487 ◽  
Author(s):  
Yan Li ◽  
David Dolphin
Keyword(s):  
Metal Complexes ◽  
Zinc Complex ◽  
Nickel Complexes ◽  
Crystallographic Analysis ◽  
Zinc Complexes ◽  
Spectral Characterization ◽  
X Ray ◽  
Almost All ◽  
C Nmr

A series of novel 1,9-diazodipyrrins (4) were readily synthesized by reacting aryldiazonium salts with 5-aryldipyrromethanes under both acidic and basic conditions. The zinc complex of 1,9-diphenylazodipyrrin (5aZn) was confirmed by X-ray crystallographic analysis, and 1,9-diazodipyrrins and their zinc and nickel complexes (5M) were characterized by 1H and 13C NMR, IR, UV–vis, and MS. All of the metal complexes absorb almost all colours of the rainbow; the absorption maximums are >650 nm and the half-band widths are over 100 nm. The fluorescence of the zinc complexes of 1,9-diphenylazodipyrrin (5aZn) and 1,9-di(2-iodophenylazo)dipyrrin (5cZn) were also explored.

Synthesis and characterization of novel azo-embedded N-confused tetraphenylporphyrin

2009 ◽  
Vol 13 (02) ◽  
pp. 215-222 ◽  
Author(s):  
Motoki Toganoh ◽  
Takayoshi Hihara ◽  
Kentaro Yonekura ◽  
Yuichi Ishikawa ◽  
Hiroyuki Furuta
Keyword(s):  
Absorption Spectrum ◽  
Effective Interaction ◽  
Coupling Reaction ◽  
Crystallographic Analysis ◽  
Synthesis And Characterization ◽  
X Ray ◽  
H Nmr ◽  
Cis Isomer ◽  
C Nmr

A unique class of azo porphyrin, 5,10,15,20-tetraphenyl-21-phenylazo-(2-aza-21-carbaporphyrin 1, in which an azophenyl group is embedded in N -confused porphyrin, was synthesized and characterized by 1 H NMR, 13 C NMR, UV-vis absorption, MS, and X-ray crystallographic analysis. Synthesis of 1 was achieved through a coupling reaction of 21-amino N -confused tetraphenylporphyrin with nitrosobenzene and subsequent deoxygenation of resulting azoxy derivative with a trioxo rhenium(VII) N -fused porphyrinato catalyst. The azo-conjugate molecule was exclusively obtained as a trans-isomer and no isomerization to the cis-isomer was observed under thermal or photoirradiation. The absorption spectrum of 1 shows a moderate red-shift due to the effective interaction between the porphyrinic π-system and the connecting azophenyl group. Upon protonation, this effect is essentially lost as a result of removing degeneracy of LUMO and LUMO+1.

Characterization of the ionic clathrate hydrate of tetra-n-butylammonium acrylate

2015 ◽  
Vol 93 (9) ◽  
pp. 954-959 ◽  
Author(s):  
Sanehiro Muromachi ◽  
Masato Kida ◽  
Satoshi Takeya ◽  
Yoshitaka Yamamoto ◽  
Ryo Ohmura
Keyword(s):  
Nmr Spectra ◽  
Clathrate Hydrate ◽  
Unit Cell ◽  
The Other ◽  
X Ray Diffraction ◽  
X Ray ◽  
Lattice Water ◽  
C Nmr ◽  
The Ideal

The ionic clathrate hydrate of tetra-n-butylammonium (TBA) acrylate was characterized using single-crystal X-ray diffraction, elemental analysis, and nuclear magnetic resonance (NMR) spectroscopy. The crystal structure of TBA acrylate was Jeffrey’s type III and tetragonal P42/n, with a 33.076(7) × 33.076(7) × 12.170(2) Å3 unit cell. The volume of the unit cell was 13315(5) Å3, which is almost twice that of the ideal structure. The TBA cation was disordered and located in two types of fused cages. Although the acrylate anion was located in a pentagonal dodecahedral cage neighboring the TBA cation, there is a residual acrylate anion that could be around the other TBA cation in the unit cell. Solid-state 13C NMR spectra showed that the TBA cation was clearly disordered at 173 K, but not at 239 K. NMR peaks from the acrylate anion were not observed at either temperature. This is probably because of the strong restriction on the acrylate anion by hydrogen bonding with the lattice water. Some of the characteristics of the anion and cation of the ionic guest incorporated in the hydrate structure have yet to be defined. Further research is needed to clarify complexation of the ionic clathrate hydrate and the ionic guest, and the resulting structure.

Crystal Forms of Semisynthetic Ergot Alkaloid Terguride

2002 ◽  
Vol 67 (4) ◽  
pp. 479-489 ◽  
Author(s):  
Michal Hušák ◽  
Bohumil Kratochvíl ◽  
Ivana Císařová ◽  
Ladislav Cvak ◽  
Alexandr Jegorov ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ergot Alkaloid ◽  
Simplified Model ◽  
Quantum Mechanical ◽  
Quantum Mechanical Calculations ◽  
X Ray Diffraction ◽  
Torsion Angles ◽  
Crystal Forms ◽  
X Ray ◽  
Independent Molecules

Two new structures of semisynthetic ergot alkaloid terguride created by unusual number of symmetry-independent molecules were determined by X-ray diffraction methods at 150 K. Form A (monoclinic, P212121, Z = 12) contains three symmetry-independent terguride molecules and two molecules of water in the asymmetric part of the unit cell. The form CA (monoclinic, P21, Z = 8) is an anhydrate remarkable by the presence of four symmetry-independent molecules in the crystal structure. Conformations of twelve symmetry-independent molecules that were found in four already described terguride structures are compared with torsion angles obtained by ab initio quantum-mechanical calculations for the simplified model of N-cyclohexyl-N'-diethylurea.

Synthesis of the novel anions [Re3H3(μ3-OR)(CO)9]− (R = Et, i-Pr, t-Bu) and x-ray characterization of [Re3H3(μ3-OEt)(CO)9](NEt4

1981 ◽  
Vol 219 (2) ◽  
pp. C23-C25 ◽  
Author(s):  
Gianfranco Ciani ◽  
Giuseppe D'Alfonso ◽  
Maria Freni ◽  
Pierfrancesco Romiti ◽  
Angelo Sironi
Keyword(s):  
The Novel ◽  
X Ray

Multinuclear Paramagnetic NMR Spectra and Solid State X-ray Crystallographic Characterization of Manganese(III) Schiff-Base Complexes

1997 ◽  
Vol 36 (22) ◽  
pp. 4968-4982 ◽  
Author(s):  
Yangzhen Ciringh ◽  
Scott W. Gordon-Wylie ◽  
Richard E. Norman ◽  
George R. Clark ◽  
Susan T. Weintraub ◽  
...  
Keyword(s):  
Schiff Base ◽  
Solid State ◽  
Nmr Spectra ◽  
Schiff Base Complexes ◽  
Paramagnetic Nmr ◽  
X Ray

6π-Tricarbonyl-Komplexe von Pyridin-Derivaten, Synthesen und Reaktionen / 6π-Tricarbonyl-Chromium Complexes of Pyridine Derivatives, Syntheses and Reactions

1984 ◽  
Vol 39 (2) ◽  
pp. 207-212 ◽  
Author(s):  
Karl Dimroth ◽  
Rüdiger Thamm ◽  
Hans Kaletsch
Keyword(s):  
Hydrogen Atom ◽  
Phosphorus Atom ◽  
Nmr Spectra ◽  
Pyridine Derivatives ◽  
Chromium Complexes ◽  
X Ray ◽  
Chromium Hexacarbonyl ◽  
Allyl Rearrangement ◽  
Tricarbonylchromium Complexes ◽  
C Nmr

New 6π-tricarbonylchromiumpyrnftne complexes 5c and 5d could be synthesized from 2,6-di-rbutyl- and 2,4,6-tri-f-butylpyridines (3c and 3d) with chromium hexacarbonyl. They are characterized by their 1H and 13C NMR Spectra and their CO-frequencies which are rather similar to those of 6π-tricarbonylchromium-2,4 ,6-triphenyl [1] or 2,4,6-trw-butyl- [2] λ3-phosphorins. When 5d is reacted with lithiumphenyl, the phenyl residue adds to C-4, giving probably compound 7, which by methanolysis and allyl rearrangement of the hydrogen atom from position 4 to position 2 affords tricarbonylchromium-2,6-di-f-butyl-4-phenyl-1,2-dihydropyridine (8) in 56% yield. The 6π-tricarbonylchromium complexes of 2,4,6-triphenyl- or 2,4,6-tn-t-butyl-λ3-phosphorins react with lithiumorganic compounds by addition only to the phosphorus atom whose reaction with methyliodide lead to tricarbonylchromium-λ5-phosphorin-ylid complexes [2], 5 d is a well crystallized compound, the X-ray analysis of the first 6π-tricarbonylchromium pyridine derivate could be performed [3] and compared with the results of the X-ray analysis of 6π-tricarbonylchromiumx 2,4,6-triphenyl-λ3-phosphorin [4]

Bis[dicarbonyl(cyclopentadienyl)ruthenium(I)] Komplexe / Bis[dicarbonyl(cyclopentadienyl)ruthenium(I)] Complexes

2002 ◽  
Vol 57 (9) ◽  
pp. 1017-1026 ◽  
Author(s):  
Herbert Schumann ◽  
Susanne Stenz ◽  
Frank Girgsdies ◽  
Stefan H. Mühle
Keyword(s):  
Single Crystal ◽  
Nmr Spectra ◽  
X Ray ◽  
Tert Butyl ◽  
New Compounds ◽  
C Nmr

Ru3(CO)12 reacts with 1-tert-butyl-2,4-cyclopentadiene (1), 1-trimethylsilyl-2,4-cyclopentadiene (2), 1-tert-butyl-3-methyl-2,4-cyclopentadiene (3), 1,3-di(tert-butyl)-2,4-cyclopentadiene (4), 1-iso-propyl-2,3,4,5-tetramethyl-2,4-cyclopentadiene (5), 1-tert-butyl-2,3,4,5-tetramethyl- 2,4-cyclopentadiene (6), 1-phenyl-2,3,4,5-tetramethyl-2,4-cyclopentadiene (7), 2,5- diphenyl-2,4-cyclopentadiene (8), or 2,3,4,5-tetraphenyl-2,4-cyclopentadiene (9) with formation of the corresponding bis[dicarbonyl(cyclopentadienyl) ruthenium(I)] complexes [RuCp# (CO)2]2 1a to 9a. The 1H and 13C NMR spectra of the new compounds 3a and 5a to 9a as well as the single crystal X-ray structures of 1a, 4a, 5a, 7a, 8a, and 9a are reported and discussed

scholarly journals Reactions of 3-(p-substituted-phenyl)-5-chloromethyl-1,2,4-oxadiazoles with KCN leading to acetonitriles and alkanes via a non-reductive decyanation pathway

2018 ◽  
Vol 14 ◽  
pp. 3011-3017
Author(s):  
Akın Sağırlı ◽  
Yaşar Dürüst
Keyword(s):  
Nmr Spectra ◽  
2D Nmr ◽  
Synthetic Route ◽  
X Ray ◽  
H Nmr ◽  
2D Nmr Spectra ◽  
Tof Ms ◽  
C Nmr

The present work describes an unfamiliar reaction of 5-(chloromethyl)-3-substituted-phenyl-1,2,4-oxadiazoles with KCN affording trisubstituted 1,2,4-oxadiazol-5-ylacetonitriles and their parent alkanes, namely, 1,2,3-trisubstituted-1,2,4-oxadiazol-5-ylpropanes. To the best of our knowledge, the current synthetic route leading to decyanated products will be the first in terms of a decyanation process which allows the transformation of trisubstituted acetonitriles into alkanes by the incorporation of KCN with the association of in situ-formed HCN and most likely through the extrusion of cyanogen which could not be detected or isolated. In addition, the plausible mechanisms were proposed for both transformations. The structures of the title compounds were identified by means of IR, 1H NMR, 13C NMR, 2D NMR spectra, TOF–MS and X-ray measurements.

Zur Darstellung und Struktur des 1.3-Dichloro-5-N.N-dimethylamino-1.3-dithia-2.4.6-triazins / Synthesis and Structure of 1,3-Dichloro-5-N,N-dimethylamino-1,3-dithia-2,4,6-triazine

1983 ◽  
Vol 38 (3) ◽  
pp. 347-349 ◽  
Author(s):  
Herbert W. Roesky ◽  
Pierre Schäfer ◽  
Mathias Noltemeyer ◽  
George M. Sheldrick
Keyword(s):  
Structure Analysis ◽  
Nmr Spectra ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cl Atoms ◽  
C Nmr

Abstract The six membered ring of composition (CH3)2NCN3S2Cl2 3 a was prepared from N,N-dimethylguanidinhydrochloride and trithiadiazindichloride. 3 a was characterized on the basis of mass, 1H, 13C NMR spectra and X-ray structure analysis. Crystals of 3 a are monoclinic, space group P21/c, with a = 660.3(6), b = 834.5(7), c = 1774.7(15) pm, β = 112.83(6)° and Z = 4. The C2N unit lies approximately in the plane of the [-CNSNSN-] ring, with both Cl atoms on the same side of the ring.

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