Crown ether analogues and their complexes. Solid-state and solution stereochemistry of dibenzo-15-crown-4 ether and its 2:2 complex with sodium iodide as studied by X-ray crystallography and NMR spectroscopic methods

1995 ◽  
pp. 707 ◽  
Author(s):  
Gerald W. Buchanan ◽  
V. Mark Reynolds ◽  
Keith Bourque ◽  
Corinne Bensimon
Keyword(s):  
Solid State ◽  
Crown Ether ◽  
Sodium Iodide ◽  
Spectroscopic Methods ◽  
X Ray ◽  
X Ray Crystallography

Synthesis and molecular structures of N,N-dialkyl-4-nitrosoaniline adducts of formally d6 metalloporphyrins of ruthenium and cobalt

2001 ◽  
Vol 05 (09) ◽  
pp. 702-707 ◽  
Author(s):  
LI CHEN ◽  
JESSE B. FOX ◽  
GEUN-BAE YI ◽  
MASOOD A. KHAN ◽  
GEORGE B. RICHTER-ADDO
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Molecular Structures ◽  
Spectroscopic Methods ◽  
X Ray ◽  
X Ray Crystallography ◽  
High Yields ◽  
Solid State Structures

Para-aminosubstituted nitrosoarenes react with Ru ( CO )( OEP ) or [ Co ( TPP )( THF )2] SbF 6 (OEP2- = 2,3,7,8,12,13,17,18-octaethylporphyrinato dianion, TPP2- = 5,10,15,20-tetraphenylporphyrinato dianion) to generate Ru ( OEP )( ONC 6 H 4 NMe 2)2 and [ Co ( TPP )( ONC 6 H 4 NR 2)2] SbF 6 ( R = Me , Et ), respectively, in fair to high yields. These N -bound nitrosoarene complexes have been characterized by spectroscopic methods. The complexes Ru ( OEP )( ONC 6 H 4 NMe 2)2 and [ Co ( TPP )( ONC 6 H 4 NMe 2)2] ClO 4 have also been characterized by single-crystal X-ray crystallography. Their structures represent the first reported solid-state structures of Ru and Co porphyrins containing C-nitroso ligands.

scholarly journals Metabolites from the Fungus Phoma sp. 7210, Associated with Aizoon Canariense

2010 ◽  
Vol 5 (8) ◽  
pp. 1934578X1000500
Author(s):  
Jingqiu Dai ◽  
Hidayat Hussain ◽  
Siegfried Dräger ◽  
Barbara Schulz ◽  
Tibor Kurtán ◽  
...  
Keyword(s):  
Solid State ◽  
Absolute Configuration ◽  
Endophytic Fungus ◽  
2D Nmr ◽  
Spectroscopic Methods ◽  
Spectral Measurements ◽  
X Ray ◽  
Mass Spectral ◽  
X Ray Crystallography ◽  
Ray Geometry

A new metabolite, 3,16-diketoaphidicolan (1), was isolated together with four known compounds: aphidicolin (2), 17-acetyl-aphidicolin (3), (+)-eupenoxide (4), and phomoxanthone A (5) from the endophytic fungus Phoma sp. The structure of the new compound 1 was determined by spectroscopic methods (mainly extensive 1D and 2D NMR experiments and by mass spectral measurements) and confirmed by X-ray crystallography. Its absolute configuration was assigned by means of the solid-state CD/TDDFT approach comparing the solid-state CD spectrum with the TDDFT-calculated one on the X-ray geometry.

scholarly journals Fusarins G–L with Inhibition of NO in RAW264.7 from Marine-Derived Fungus Fusarium solani 7227

Marine Drugs ◽  
2021 ◽  
Vol 19 (6) ◽  
pp. 305
Author(s):  
Guangyuan Luo ◽  
Li Zheng ◽  
Qilin Wu ◽  
Senhua Chen ◽  
Jing Li ◽  
...  
Keyword(s):  
Fusarium Solani ◽  
2D Nmr ◽  
Inflammatory Activity ◽  
Raw264.7 Cells ◽  
Spectroscopic Methods ◽  
X Ray ◽  
X Ray Crystallography ◽  
Structure Activity ◽  
Ic50 Values ◽  
New Compounds

Six new fusarin derivatives, fusarins G–L (1–6), together with five known compounds (5–11) were isolated from the marine-derived fungus Fusarium solani 7227. The structures of the new compounds were elucidated by means of comprehensive spectroscopic methods (1D and 2D NMR, HRESIMS, ECD, and ORC) and X-ray crystallography. Compounds 5–11 exhibited potent anti-inflammatory activity by inhibiting the production of NO in RAW264.7 cells activated by lipopolysaccharide, with IC50 values ranging from 3.6 to 32.2 μM. The structure–activity relationships of the fusarins are discussed herein.

scholarly journals A Mixed-metal Mixed-halide Complex Prepared from Zerovalent Copper and Lead Salts: Solution and Solid-state Chemistry

1999 ◽  
Vol 23 (11) ◽  
pp. 670-671
Author(s):  
Larisa A. Kovbasyuk ◽  
Olga Yu. Vassilyeva ◽  
Vladimir N. Kokozay ◽  
Wolfgang Linert ◽  
Paul R. Raithby
Keyword(s):  
Solid State ◽  
Direct Interaction ◽  
Solid State Chemistry ◽  
X Ray ◽  
Mixed Metal ◽  
X Ray Crystallography ◽  
Halide Complex ◽  
Layer Arrangement ◽  
Lead Salts

The mixed-metal mixed-halide complex [CuPbBrlL2]2 has been prepared by the direct interaction of zerovalent copper with lead halides and 2-dimethylaminoethanol (HL) in dmso and has been characterized by X-ray crystallography; the structure shows a layer arrangement of the tetranuclear metal units through the μ3-halogen bridging.

Bis(1-phenyl-1-propyne) complexes of tungsten(II): crystal structures of [WI2(CO)(NCR)(η2-MeC2Ph)2] (R = Me, Et, or Ph)

2001 ◽  
Vol 79 (3) ◽  
pp. 263-271
Author(s):  
Paul K Baker ◽  
Michael GB Drew ◽  
Deborah S Evans
Keyword(s):  
Carbon Monoxide ◽  
Solid State ◽  
Crystal Structures ◽  
Octahedral Geometry ◽  
X Ray ◽  
X Ray Crystallography ◽  
Alkyne Complexes ◽  
First Time

Reaction of [WI2(CO)3(NCMe)2] with two equivalents of 1-phenyl-1-propyne (MeC2Ph) in CH2Cl2, and in the absence of light, gave the bis(1-phenyl-1-propyne) complex [WI2(CO)(NCMe)(η2-MeC2Ph)2] (1) in 77% yield. Treatment of equimolar quantities of 1 and NCR (R = Et, i-Pr, t-Bu, Ph) in CH2Cl2 afforded the nitrile-exchanged products, [WI2(CO)(NCR)(η2-MeC2Ph)2] (2-5) (R = Et (2), i-Pr (3), t-Bu (4), Ph (5)). Complexes 1, 2, and 5 were structurally characterized by X-ray crystallography. All three structures have the same pseudo-octahedral geometry, with the equatorial sites being occupied by cis and parallel alkyne groups, which are trans to the cis-iodo groups. The trans carbon monoxide and acetonitrile ligands occupy the axial sites. In structures 1 and 2, the methyl and phenyl substituents of the 1-phenyl-1-propyne ligands are cis to each other, whereas for the bulkier NCPh complex (5), the methyl and phenyl groups are trans to one another. This is the first time that this arrangement has been observed in the solid state in bis(alkyne) complexes of this type.Key words: bis(1-phenyl-1-propyne), carbonyl, nitrile, diiodo, tungsten(II), crystal structures.

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

Solid state stereochemistry of crown ethers: X-ray crystal structure and 13C NMR studies of the LiNCS complex of 1,4,7,11-tetraoxacyclotetradecane

2000 ◽  
Vol 78 (3) ◽  
pp. 316-321
Author(s):  
G W Buchanan ◽  
A B Driega ◽  
G PA Yap
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crown Ether ◽  
13C Nmr ◽  
Title Complex ◽  
Nmr Studies ◽  
Nmr Spectrum ◽  
X Ray ◽  
Large Amplitude Motion ◽  
C Nmr

The title complex is asymmetric in the crystal due to the spatial orientation of the NCS function. The space group has been determined to be P21 with a = 9.496(3), b = 8.736(3), c = 9.676(3) Å, β = 117.859(5)°, and Z = 2. The solid state 13C NMR spectrum is consistent with the lack of symmetry in the crystal and there is little evidence for large amplitude motion in the macrocycle as determined from the dipolar dephased spectrum.Key words: macrocyclic crown ether, lithium complex.

scholarly journals Simple Methylcadmium Alkoxides

2007 ◽  
Vol 62 (10) ◽  
pp. 1339-1342 ◽  
Author(s):  
Surajit Jana ◽  
Tania Pape ◽  
Norbert W. Mitzel
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Molecular Formula ◽  
Equimolar Ratio ◽  
X Ray ◽  
X Ray Crystallography ◽  
Elemental Analyses ◽  
Solid State Structures ◽  
Structural Aspects ◽  
C Nmr

The reaction of dimethylcadmium with alcohols R-OH in equimolar ratio leads to the formation of tetrameric methylcadmium alkoxides with molecular formula [(MeCd)4 (OR)4] [R = Me (1), Et (2) and iPr (3)]. These compounds have been characterised by 1H, 13C NMR and IR spectroscopy, by mass spectrometry, elemental analyses and by X-ray crystallography (for 2 and 3). The solid state structures show distorted cubane-type aggregates with Cd4O4 cores. The structural aspects and the spectroscopic characterisations of these compounds are discussed.

Synthesis and characterization of the binuclear diamido titanium chalcogenides [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, Te)

2002 ◽  
Vol 80 (11) ◽  
pp. 1524-1529 ◽  
Author(s):  
Tianle Zhang ◽  
Warren E Piers ◽  
Masood Parvez
Keyword(s):  
Solid State ◽  
Key Words ◽  
Synthesis And Characterization ◽  
Catalyst Precursor ◽  
Tellurium Atom ◽  
Titanium Complex ◽  
X Ray ◽  
X Ray Crystallography ◽  
Atom Source

Reaction of McConville's chelating amido titanium complex [(Ar)NCH2CH2CH2N(Ar)]Ti(CH3)2 (Ar = 2,6-i-Pr2C6H3) with either elemental Se or the tellurium atom source Te=PBu3 resulted in the formation of bis-µ-chalcogenido dimers [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, 2; Te, 3) with concommitant loss of EMe2. The dimers 2 and 3 were characterized spectroscopically and via X-ray crystallography. The two compounds are isostructural in the solid state. The tellurido dimer 3 may also be synthesized by reduction of the diamido dichloride [(Ar)NCH2CH2CH2N(Ar)]2TiCl2 with Na–Hg amalgam followed by treatment with Te=PBu3. This dimer is unreactive toward further Te=PBu3 or stannanes such as HSnBu3. Unlike decamethyltitanocene derivatives, the diamido complex is not an effective catalyst precursor for the heterohydrodecoupling of Te=PBu3 and HSnBu3.Key words: diamido titanium complexes, selenides, tellurides.

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