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 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.

Synthesis of ReItricarbonyl complexes with various sulfur- and oxygen-donating ligands: crystal structures of two ReIdinuclear structures bridged by S atoms

2018 ◽  
Vol 74 (10) ◽  
pp. 1116-1122
Author(s):  
Pheello I. Nkoe ◽  
Hendrik G. Visser ◽  
Chantel Swart ◽  
Alice Brink ◽  
Marietjie Schutte-Smith
Keyword(s):  
Hydrogen Bond ◽  
Intermolecular Hydrogen Bond ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
Pyridine Ligand ◽  
X Ray ◽  
Hydrogen Bond Interactions ◽  
Mononuclear Complexes

The synthesis and characterization of two dinuclear complexes, namelyfac-hexacarbonyl-1κ3C,2κ3C-(pyridine-1κN)[μ-2,2′-sulfanediyldi(ethanethiolato)-1κ2S1,S3:2κ3S1,S2,S3]dirhenium(I), [Re2(C4H8S3)(C5H5N)(CO)6], (1), and tetraethylammoniumfac-tris(μ-2-methoxybenzenethiolato-κ2S:S)bis[tricarbonylrhenium(I)], (C8H20N)[Re2(C7H7OS)3(CO)6], (2), together with two mononuclear complexes, namely (2,2′-bithiophene-5-carboxylic acid-κ2S,S′)bromidotricarbonylrhenium(I), (3), and bromidotricarbonyl(methyl benzo[b]thiophene-2-carboxylate-κ2O,S)rhenium(I), (4), are reported. Crystals of (1) and (2) were characterized by X-ray diffraction. The crystal structure of (1) revealed two Re—S—Re bridges. The thioether S atom only bonds to one of the ReImetal centres, while the geometry of the second ReImetal centre is completed by a pyridine ligand. The structure of (2) is characterized by three S-atom bridges and an Re...Re nonbonding distance of 3.4879 (5) Å, which is shorter than the distance found for (1) [3.7996 (6)/3.7963 (6) Å], but still clearly a nonbonding distance. Complex (1) is stabilized by six intermolecular hydrogen-bond interactions and an O...O interaction, while (2) is stabilized by two intermolecular hydrogen-bond interactions and two O...π interactions.

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.

Structural Diversity of Hydrogen-Bonded Networks of [Co(NH3)6]3+ Complex Cations and Acetylenedicarboxylic Acid Anions

2014 ◽  
Vol 69 (3) ◽  
pp. 277-288 ◽  
Author(s):  
Rüdiger W. Seidel ◽  
Richard Goddard ◽  
Verena Gramm ◽  
Uwe Ruschewitz
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Structural Diversity ◽  
Crystalline Material ◽  
X Ray Diffraction ◽  
Slow Cooling ◽  
Unknown Compound ◽  
X Ray ◽  
Acetylenedicarboxylic Acid

2011The crystal structure of [Co(NH3)6](ADC)(HADC) · 2H2O (1) (ADC2- =acetylenedicarboxylate) (P21=n, Z = 4) was mistakenly described as containing the [Co(H2O)6]3+ ion [I. Stein, U. Ruschewitz, Z. Naturforsch. , 66b, 471 - 478]. A revision is reported. While attempting to reproduce 1, we isolated phase-pure crystalline material of [Co(NH3)6]Cl2(HADC) · H2O (2), the crystal structure of which was also reported in the article above. Upon standing in the aqueous mother liquor at room temperature for several days, the needle-shaped crystals of 2disappear, while blockshaped crystals of the formerly unknown compound [Co(NH3)6](ADC)(HADC) (3) grow. Satellite peaks in the X-ray diffraction frames indicate that the crystal structure is incommensurately modulated. Dissolving crystals of 3 in water at elevated temperature leads to plate-shaped crystals of the new compound [Co(NH3)6]2(ADC)3 · 3H2O (4) upon slow cooling to room temperature. Compounds 2- 4 were investigated by elemental analysis, powder X-ray diffraction and infrared spectroscopy. Structural characterization of 4 by single-crystal X-ray analysis was also achieved (P1̅ , Z = 2). Complex 1, however, could not be reproduced

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.

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