Synthesis and characterization of a hexaphyrin(1.0.1.0.0.0) bearing both meso- and β-substituents

2007 ◽  
Vol 11 (04) ◽  
pp. 287-293 ◽  
Author(s):  
Jonathan L. Sessler ◽  
Patricia J. Melfi ◽  
Vincent M. Lynch
Keyword(s):  
Crystal Structure ◽  
Ring Current ◽  
Spectroscopic Studies ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Planar Conformation ◽  
Hydrogen Bound

The synthesis of an isoamethyrin-type expanded porphyrin bearing both meso- and β-substituents is presented. The diprotonated form of this macrocycle was characterized by conventional spectroscopic means and via a single crystal X-ray diffraction analysis. This species is observed to adopt a planar conformation in the solid state. Nonetheless, the inner ring current, as inferred from 1 H NMR spectroscopic studies, is found to be severely diminished as compared to isoamethyrin, by the presence of the two meso-phenyl moieties. A second crystal structure, in which a molecule of water is hydrogen-bound to a pyrrole NH , was also solved.

Oxazoline chemistry — Part IV: Synthesis and characterization of oxazoline complexes of the zinc halides

2003 ◽  
Vol 81 (12) ◽  
pp. 1482-1491 ◽  
Author(s):  
Tosha M Barclay ◽  
Ignacio del Río ◽  
Robert A Gossage ◽  
Sarah M Jackson
Keyword(s):  
Crystal Structure ◽  
Structural Diversity ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
Zinc Compounds ◽  
X Ray ◽  
H Nmr ◽  
Oxazoline Ligands

The synthesis and characterization of 11 zinc halide derivatives that contain monodentate oxazoline ligands is described. The treatment of ether solutions of [ZnX2] (X = Cl, Br, I) with 2-aryl- or 2-methyl-2-oxazolines results in the formation of mildly hygroscopic complexes of the general formulae [ZnX2(ox)2] (ox = 2-methyl-2-oxazoline (1), 2,4,4-trimethyl-2-oxazoline (2), 2-phenyl-2-oxazoline (3), or 4,4-dimethyl-2-phenyl-2-oxazoline (4)), except in the case of ZnI2, which does not form an isolable complex — likely for steric reasons — with oxazoline 4. Treatment of [ZnBr2(4)2] with 1 reveals (1H NMR) that 1 only sluggishly displaces coordinated 4 at temperatures below 50 °C. The structural characterization, via single crystal X-ray diffraction, of six of the complexes, viz. [ZnI2(1)2], [ZnI2(2)2], [ZnX2(3)2] (X = Cl, Br, or I), and [ZnBr2(4)2], is also reported. All of these structurally characterized complexes are mononuclear zinc compounds with an overall distorted tetrahedral arrangement of the two halide and two oxazoline ligands around the zinc metal centre. The oxazoline series of complexes reported herein show little structural diversity, a facet which is in contrast to their substituted pyridine analogues.Key words: oxazoline, zinc, X-ray crystal structure, coordination complex, NMR spectroscopy, Zn(II).

Synthesis and Characterization of a New Copper(II) Complex with Nadolol, an Aminoalcoholic Beta-blocker. Crystal Structure of Na[Cu(nadololate)(CO3)] · H2O

2008 ◽  
Vol 63 (5) ◽  
pp. 543-547 ◽  
Author(s):  
Inés Viera ◽  
Laura Domínguez ◽  
Javier Ellena ◽  
María H. Torre
Keyword(s):  
Crystal Structure ◽  
Vibrational Spectroscopy ◽  
Copper Complex ◽  
Beta Blocker ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Spectroscopy Analysis ◽  
X Ray

This work reports the synthesis and characterization of a new copper complex with nadolol, a betablocker aminoalcohol. The stoichiometry found was Na[Cu(nadololate)(CO3)] · H2O. Electronic and vibrational spectroscopy analysis was performed, and the crystal structure of Na[Cu(nadololate)-(CO3)] · H2O was determined by X-ray diffraction.

Synthesis and Characterization of Co Nanoparticles by Solventless Thermal Decomposition

2007 ◽  
Vol 119 ◽  
pp. 71-74 ◽  
Author(s):  
Yan Li ◽  
Xiao Li Zhang ◽  
Young Hwan Kim ◽  
Young Soo Kang
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Synthesis And Characterization ◽  
Vibrating Sample Magnetometer ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Structure Of Nanoparticles ◽  
Co Nanoparticles

Co nanoparticles were synthesized via a solventless thermal decomposition of Co2+-oleate2. The crystalline structure is strongly affected by the thermal treatment of the Co nanoparticles. Further, the annealing also results in the decomposition of surfactant around Co particles. The size of nanoparticles was confirmed by transmission electron microscopy (TEM). The crystal structure of nanoparticles was characterized by X-ray diffraction pattern (XRD). The magnetic properties were characterized by vibrating sample magnetometer (VSM).

Synthesis and Characterization of ALaFeNi0.5W0.5O6 (A= Sr or Ca), a New Structure Distorted Double Perovskite

2013 ◽  
Vol 717 ◽  
pp. 133-138
Author(s):  
A. Awad Allah ◽  
M. Elhadi ◽  
O.A. Yassien
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Double Perovskite ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Absorption Bands ◽  
X Ray ◽  
Perovskite Materials ◽  
Ftir Spectrometer

The crystal structure of both samples has been solved by powder X-ray diffraction, data in the tetragonal space group I4/m (a= b= 5.55182 Å, c =7.86955 A0) for SrLaFeNi0.5W0.5O6sample and (a=b= 5.49129Å, c= 7.82233Å) for CaLaFeNi0.5W0.5O6 sample, and shows an almost perfect ordering between Ni2+ and W5+ cations at the B-site of the perovskite structure. The FTIR spectrometer used of the powders showed that the spectra of both are very similar, showing two strong and well-defined absorption bands, typical of perovskite materials.

Synthesis and Electrochemistry of Aluminum Porphycenes: Crystal and Molecular Structure of Methyl-σ-Bonded Aluminum Etioporphycene

1997 ◽  
Vol 01 (02) ◽  
pp. 109-119 ◽  
Author(s):  
ROGER GUILARD ◽  
VIRGINIE PICHON-PESME ◽  
HASSANE LACHEKAR ◽  
CLAUDE LECOMTE ◽  
ALLY M. AUKAULOO ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Structural Data ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Axial Ligands ◽  
Uv Visible

The synthesis and characterization of three monomeric aluminum porphycenes with anionic or σ-bonded axial ligands is reported. The investigated compounds are represented as ( EtioPc ) Al ( CH 3) and ( EtioPc ) AlX where EtioPc represents the dianion of etioporphycene and X = Cl − or OH −. Each synthesized complex was characterized by mass spectrometry. 1 H NMR, IR and UV-visible spectroscopies as well as by electrochemistry. Comparisons are made between the properties of complexes in the aluminum etioporphycene series and related chloro- or methyl σ-bonded Al ( III ) porphyrins containing octaethylporphyrin ( OEP ) or tetraphenylporphyrin ( TPP ) macrocycles. Comparisons are also made between the currently investigated compounds and a previously reported Al ( III ) μ-oxo dimer, [( EtioPc ) Al ]2 O . In addition, the crystal and molecular structure of ( EtioPc ) Al ( CH 3) was determined by X-ray diffraction. The molecular structure of this methyl-σ-bonded aluminum etioporphycene provides the first structural data for an aluminum porphycene compound. The aluminum(III) atom in ( EtioPc ) Al ( CH 3) is pentacoordinated and is located 0.54 Å from the plane of the four N -nitrogens.

Synthesis and Characterization of a Dumbbell-Shaped Polyrotaxane Based on Polytetrahydrofuran bis(3-aminopropyl) Terminated and α-Cyclodextrins Using Polyamidoamine (PAMAM) Dentrimers as Bulky Stoppers

2015 ◽  
Vol 1094 ◽  
pp. 41-48
Author(s):  
Ri Min Cong ◽  
Huai Qing Yu ◽  
Yan Gong Yang ◽  
Si Yi Yang ◽  
Jiao Li ◽  
...  
Keyword(s):  
Thermogravimetric Analysis ◽  
Inclusion Complex ◽  
Inclusion Complexes ◽  
Synthesis And Characterization ◽  
Wide Angle ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Channel Type

A dumbbell-shaped polyrotaxane based on polytetrahydrofuran bis (3-aminopropyl) terminated and α-cyclodextrins using polyamidoamine (PAMAM) dentrimers as bulky stoppers was successfully prepared. The1H NMR results show that the peaks of α-CDs in these polyrotaxanes are broadened compared with pure α-CDs. Wide-angle X-ray diffraction (XRD) measurements of the resulting polyrotaxanes suggest to produce a channel-type crystalline structure of inclusion complex. Thermogravimetric analysis (TGA) of the resultant polyrotaxanes show that α-CDs are significantly stabilized by the formation of the inclusion complexes.

Synthesis and Characterization of a Cubic Iron Hydroxy Boracite

2011 ◽  
Vol 66 (2) ◽  
pp. 107-114 ◽  
Author(s):  
Stephanie C. Neumair ◽  
Johanna S. Knyrim ◽  
Oliver Oeckler ◽  
Reinhard Kaindl ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
High Temperature ◽  
Single Crystals ◽  
Room Temperature ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Pressure High Temperature

The cubic iron hydroxy boracite Fe3B7O13OH・1.5H2O was synthesized from Fe2O3 and B2O3 under high-pressure/high-temperature conditions of 3 GPa and 960 °C in a modified Walker-type multianvil apparatus. The crystal structure was determined at room temperature by X-ray diffraction on single crystals. It crystallizes in the cubic space group F4̄3c (Z = 8) with the parameters a = 1222.4(2) pm, V = 1.826(4) nm3, R1 = 0.0362, and wR2 = 0.0726 (all data). The B-O network is similar to that of other cubic boracites.

Notizen: Synthesis and Characterization of Nadorite: PbSbO2Cl

2002 ◽  
Vol 57 (3) ◽  
pp. 360-362 ◽  
Author(s):  
Yetta Porter ◽  
P. Shiv Halasyamani
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thermogravimetric Data

AbstractThe first labortory synthesis and characterization of the mineral Nadorite, PbSbO2Cl, is reported. The material was synthesized by combining PbCl2, PbO and Sb2O3. Powder X-ray diffraction data on the polycrystalline product is consistent with the previously reported crystal structure on the mineral. Infrared and thermogravimetric data are also present.

Synthesis and Crystal Structure of 4-[5-(2-Bromophenyl)-1,3,4-Thiadiazol-2-Ylthio]-2-(trifluoromethyl)thieno[2,3-d]pyrimidine

2014 ◽  
Vol 887-888 ◽  
pp. 703-706
Author(s):  
Ping Yang ◽  
Hui Gao ◽  
Yao Nie ◽  
Zhen Zeng ◽  
Jin Shun Zhao ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Trifluoroacetic Acid ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
H Nmr ◽  
Planar Conformation ◽  
Step Procedure ◽  
Title Molecule

4-[5-(2-Bromophenyl)-1,3,4-thiadiazol-2-ylthio]-2-(trifluoromethyl)thieno[2,3-d]pyrimidine was synthesized by a facile three-step procedure, including the cyclization of 2-aminothiophene-3-carbonitrile with trifluoroacetic acid, chlorination and nucleophilic substitution reaction. This protocol offers such advantages as mild reaction conditions, simple purification and good yields. The structure of the product was characterized by 1H NMR, MS, elemental analysis and single-crystal X-ray diffraction. X-Ray diffraction analysis reveals that the title molecule essentially assumes a planar conformation except for the F atoms.

scholarly journals Synthesis and characterization of π–extended “earring” subporphyrins

2018 ◽  
Vol 14 ◽  
pp. 1956-1960 ◽  
Author(s):  
Haiyan Guan ◽  
Mingbo Zhou ◽  
Bangshao Yin ◽  
Ling Xu ◽  
Jianxin Song
Keyword(s):  
Single Crystal ◽  
Aromatic Ring ◽  
Nmr Spectra ◽  
Ring Current ◽  
Synthesis And Characterization ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Single Crystal Structures

A π-extended “earring” subporphyrin 3 was synthesized from β,β′-diiodosubporphyrin and diboryltripyrrane via a Suzuki–Miyaura coupling and following oxidation. Its Pd complex 3Pd was also synthesized and both of the compounds were fully characterized by 1H NMR, MS and X-ray single crystal diffraction. The 1H NMR spectra and single crystal structures revealed that aromatic ring current did not extend to the “ear” in both of the two compounds. Their UV–vis/NIR spectra were recorded and the absorption of both compounds is extended to the NIR region and that the absorption of 3Pd is further red-shifted and more intense.

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