scholarly journals Synthesis, Characterization, and Crystal Structure of Pyridinium Tetrakis{1-trifluoromethyl-3-(1′-pyreno)-1,3-propanedionato}lanthanate(III) Complex

2014 ◽  
Vol 2014 ◽  
pp. 1-6
Author(s):  
Tetsuji Moriguchi ◽  
Kenji Yoza ◽  
Akihiko Tsuge
Keyword(s):  
Ligand Exchange ◽  
Fast Atom Bombardment ◽  
Proton Nuclear Magnetic Resonance ◽  
Resonance Spectroscopy ◽  
X Ray Diffraction ◽  
Visible Spectroscopy ◽  
X Ray ◽  
Mild Conditions ◽  
Polycyclic Aromatic ◽  
Halide Ligand

The reaction of 1-trifluoromethyl-3-(1′-pyreno)-1,3-propanedione with lanthanum(III) trichloride in the presence of pyridine leads to halide ligand exchange, yielding a novel pyridinium tetrakis{1-trifluoromethyl-3-(1′-pyreno)-1,3-propanedionato}lanthanate(III) complex with four polycyclic aromatic hydrocarbon moieties. This reaction easily proceeds under mild conditions (25°C, 24 h) producing the complex in a 90% isolated yield. The complex was characterized by infrared spectroscopy, proton nuclear magnetic resonance spectroscopy, and positive fast atom bombardment mass spectrometry, and its precise structure was determined by single crystal X-ray diffraction. Ultraviolet-visible spectroscopy, fluorescence spectroscopy, and X-ray analysis demonstrated that the four pyrene moieties were independently oriented.

An unusual reaction of a bridged triterpenoid α-diketone with acetic anhydride

1991 ◽  
Vol 56 (12) ◽  
pp. 2917-2935 ◽  
Author(s):  
Eva Klinotová ◽  
Václav Křeček ◽  
Jiří Klinot ◽  
Miloš Buděšínský ◽  
Jaroslav Podlaha ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Nmr Spectroscopy ◽  
Acetic Anhydride ◽  
Spectral Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mild Conditions ◽  
Condensation Products ◽  
Unsaturated Lactones ◽  
C Nmr

3β-Acetoxy-21,22-dioxo-18α,19βH-ursan-28,20β-olide (IIIa) reacts with acetic anhydride in pyridine under very mild conditions affording β-lactone IVa and γ-lactones Va and VIIa as condensation products. On reaction with pyridine, lactones Va and VIIa undergo elimination of acetic acid to give unsaturated lactones VIIIa and IXa, respectively. Similarly, the condensation of 20β,28-epoxy-21,22-dioxo-18α,19βH-ursan-3β-yl acetate (IIIb) with acetic anhydride leads to β-lactone IVb and γ-lactone Vb; the latter on heating with pyridine affords unsaturated lactone VIIIb and 21-methylene-22-ketone Xb. The structure of the obtained compounds was derived using spectral methods, particularly 1H and 13C NMR spectroscopy; structure of lactone IVa was confirmed by X-ray diffraction.

Tris(dimethylphenylphosphine)ruthenium(0) Complexes of n4-Coordinated Polycyclic Aromatic Hydrocarbons

2000 ◽  
Vol 53 (6) ◽  
pp. 507 ◽  
Author(s):  
Martin A. Bennett ◽  
Mark Bown ◽  
David C. R. Hockless
Keyword(s):  
Coordination Geometry ◽  
Crystal Data ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Tertiary Phosphine ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Polycyclic Aromatic ◽  
R Value ◽  
Axial Site

From the reaction of [Ru2Cl3(PMe2Ph)6] Cl with the appropriate radical anions, yellow complexes of general formula [Ru(PMe2Ph)3(η4-arene)] [arene = naphthalene (C10H8) (1), anthracene (C14H10) (2), and triphenylene (C18H12) (3)] have been isolated in poor yield and characterized by elemental analysis, n.m.r. (1H, 13C, 31P) spectroscopy and single-crystal X-ray diffraction. Crystal data: (1), monoclinic, C2/c, a 31.096(8), b 12.012(4), c 17.078(8) Å, β 104.41(3)˚, V 6178(4) Å3, ? 8, refined to final R value of 0.032 with use of 3641 reflections [I > 3σ(I)]; (2), monoclinic, C2/c, a 55.909(4), b 14.348(5), c 17.573(5) Å, β 105.41(1)˚, V 13590(6) Å3, Z 16 (two molecules per asymmetric unit), refined to final R value of 0.049 with use of 7770 reflections [I > 3σ(I)]; (3), mono-clinic, Pn, a 9.377(3), b 12.229(3), c 15.975(3) Å, β 103.51(2)˚, V 1781.2 (7) Å3, Z 2, refined to final R value of 0.026 with use of 2830 reflections [I > 3σ(I)]. In each case, coordination of the zerovalent metal fragment Ru(PMe2Ph)3 to the diene section of one of the terminal rings causes the aromatic molecule to be folded by c. 40˚ at the outer carbon atoms of the diene. The coordination geometry about ruthenium is approximately square pyramidal, with the diene and two tertiary phosphines in the equatorial plane and the remaining tertiary phosphine in the axial site.

Organic Crystals in the Tracheids of Torreya Yunnanensis

IAWA Journal ◽  
1996 ◽  
Vol 17 (4) ◽  
pp. 393-403 ◽  
Author(s):  
Yuki Kondo ◽  
Tomoyuki Fujii ◽  
Yoshioki Hayashi ◽  
Atsushi Kato
Keyword(s):  
Phase Contrast ◽  
Growth Ring ◽  
Uv Spectra ◽  
Resonance Spectroscopy ◽  
Organic Crystals ◽  
X Ray Diffraction ◽  
Cinnamic Aldehyde ◽  
X Ray ◽  
Polarised Light ◽  
Contrast Microscopy

Organic crystals were found in tracheid lumina of some samples of Torreya yunnanensis Chen ' L. K. Fu imported from Yunnan, China. Tracheids with crystals were found in short to long tangential bands along the growth ring boundaries. Because the crystals were rapidly dissolved with ethanol and xylene, cross and tangential sections were mounted in de-ionized water without staining and observed by biological, polarised light, and phase-contrast microscopy. The crystals were sublimated under vacuum during routine sample preparation for conventional SEM and only the peripheral parts remained. With the aid of low vacuum-SEM and modified cryo-SEM procedure, the shape of the crystals was revealed. Some were styloid and large enough to fill tracheid lumina, while others were stacked appearing as slates filling tracheid lumina. X-ray diffraction applied to sections and isolated crystals showed that they were single crystals and orientated along the cell wall. UV spectra on isolated crystals and methanol dissolution of crystals suggested that they were composed of phenolic compounds. Crystals that were recrystallized from methanol were analysed by 1H and l3C nuclear magnetic resonance spectroscopy. These two techniques revealed that the major and minor components were o-methoxy cinnamic acid and o-methoxy cinnamic aldehyde.

scholarly journals Bio Synthesis and Characterization of Silver Nanoparticles Using Lagenaria siceraria Leaf Extract and their Antibacterial Activity

2014 ◽  
Vol 38 ◽  
pp. 35-45 ◽  
Author(s):  
B. Anandh ◽  
A. Muthuvel ◽  
M. Emayavaramban
Keyword(s):  
Silver Nanoparticles ◽  
Leaf Extract ◽  
Face Centered Cubic ◽  
Lagenaria Siceraria ◽  
Human Pathogens ◽  
X Ray Diffraction ◽  
Visible Spectroscopy ◽  
X Ray ◽  
Ft Ir ◽  
Uv Visible

The present investigation demonstrates the formation of silver nanoparticles by the reduction of the aqueous silver metal ions during exposure to the Lagenaria siceraria leaf extract. The synthesized AgNPs have characterized by UV-visible spectroscopy, X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) techniques. AgNPs formation has screened by UV-visible spectroscopy through colour conversion due to surface plasma resonance band at 427 nm. X-ray diffraction (XRD) confirmed that the resulting AgNPs are highly crystalline and the structure is face centered cubic (fcc). FT-IR spectrum indicates the presence of different functional groups present in the biomolecules capping the nanoparticles. Further, inhibitory activity of AgNPs and leaf extract were tested against human pathogens like gram-pastive (Staphylococcus aureus, Bacillus subtilis), gram-negative (Escherichia coli and Pseudomonas aeruginosa). The results indicated that the AgNPs showed moderate inhibitory actions against human pathogens than Lagenaria siceraria leaf extract, demonstrating its antimicrobial value against pathogenic diseases

Carboxyl graphene reinforced melamine-based polyamide nanocomposites

2021 ◽  
pp. 089270572110514
Author(s):  
Himanshu V Madhad ◽  
Dilip V Vasava
Keyword(s):  
Electron Microscopy ◽  
Decomposition Temperature ◽  
Differential Scanning Calorimetric ◽  
X Ray Diffraction ◽  
One Pot ◽  
X Ray ◽  
Mild Conditions ◽  
Thermal Stability Of ◽  
Infrared Techniques ◽  
Scanning Electron

Over the years, various types of techniques have been used for the synthesis of nanocomposites. In this work, melamine-based polyamide (PA) was synthesized using a one-pot polycondensation method under mild conditions. carboxyl graphene (CG)/PA nanocomposites (CGMPA) were prepared by CG nanofiller loadings of 1, 3, and 5 wt.% via delamination/adsorption approach. The prepared CGMPA nanocomposites were characterized using different analyses, such as Fourier transform infrared techniques (FTIR), field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), differential scanning calorimetric (DSC), and thermogravimetric analysis (TGA). The effects of the CG on the thermal properties of the CGMPA nanocomposites were significant. The results showed that the melting temperature (Tm) of neat PA and CGMPA were increased from 378°C to 393°C suggested better dispersion of CG in PA matrix. The decomposition temperature of PA was increased from 451°C to 463°C in CGMPA nanocomposites indicates the better thermal stability of PA matrix by addition of CG.

XRD investigation of thermal degradation of some gamma-irradiated polyethylene terephthalate samples

2019 ◽  
Vol 33 (12) ◽  
pp. 1950111 ◽  
Author(s):  
Mihai Todica ◽  
Zoltan Kovacs-Krauss ◽  
Carmen Niculaescu ◽  
Marieta Mureşan-Pop
Keyword(s):  
Thermal Treatment ◽  
Polyethylene Terephthalate ◽  
Structural Changes ◽  
Diffraction Method ◽  
Resonance Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Before And After ◽  
Gamma Irradiated ◽  
Different Doses

The modification of local structure of some commercial polyethylene terephthalate (PET) samples, gamma irradiated at different doses, was investigated by X-ray diffraction method before and after thermal treatment. Before the thermal treatment, the samples exposed to different doses of gamma radiations, does not show noticeable structural changes. However, the gamma exposure affects the thermal behavior of samples submitted to melting–cooling process. These modifications have been highlighted by X-ray diffraction, and confirmed also by thermal analysis and electron spin resonance spectroscopy.

scholarly journals Synthesis, Crystal Structure, and Properties of a Zn(II) Coordination Polymer Based on a Difunctional Ligand Containing Triazolyl and Carboxyl Groups

Crystals ◽  
2018 ◽  
Vol 8 (11) ◽  
pp. 424 ◽  
Author(s):  
Jia-Le Li ◽  
Wei-Dong Li ◽  
Zi-Wei He ◽  
Shuai-Shuai Han ◽  
Shui-Sheng Chen
Keyword(s):  
Coordination Polymer ◽  
Weak Interactions ◽  
Layer Structure ◽  
Three Dimensional ◽  
Stacking Interactions ◽  
Structure And Properties ◽  
X Ray Diffraction ◽  
Visible Spectroscopy ◽  
X Ray ◽  
Uv Visible

A new compound, namely, [Zn(L)2]n (1) was obtained by the reaction of 2-methyl-4-(4H-1,2,4-triazol-4-yl) benzoic acid (HL) with ZnSO4·7H2O, and the compound was characterized by single-crystal X-ray diffraction, infrared spectroscopy, elemental analysis, powder X-ray diffraction (PXRD), and thermogravimetric analysis. The linear HL ligands were deprotonated to be L− anions and act as two-connectors to link Zn2+ to form a two-dimensional (2D) lay structure with (4, 4) topology. The large vacancy of 2D framework allows another layer structure to interpenetrate, resulting in the formation of 2D + 2D → 2D parallel interpenetration in 1. The weak interactions, such as hydrogen bonding and π–π stacking interactions, connect the adjacent 2D layers into a three-dimensional (3D) coordination polymer. The solid-state UV-visible spectroscopy and luminescent property have also been studied.

scholarly journals Novel H-Bonded Synthons in Copper Supramolecular Frameworks with Aminoethylpiperazine-Based Ligands. Synthesis, Structure and Catalytic Activity

Materials ◽  
2020 ◽  
Vol 13 (23) ◽  
pp. 5435
Author(s):  
Oksana V. Nesterova ◽  
Armando J. L. Pombeiro ◽  
Dmytro S. Nesterov
Keyword(s):  
Reaction Mechanisms ◽  
Active Catalyst ◽  
Single Point ◽  
Organic Ligand ◽  
Schiff Base Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mild Conditions ◽  
Butyl Peroxide ◽  
Supramolecular Networks

New Schiff base complexes [Cu2(HL1)(L1)(N3)3]∙2H2O (1) and [Cu2L2(N3)2]∙H2O (2) were synthesized. The crystal structures of 1 and 2 were determined by single-crystal X-ray diffraction analysis. The HL1 ligand results from the condensation of salicylaldehyde and 1-(2-aminoethyl)piperazine, while a new organic ligand, H2L2, was formed by the dimerization of HL1 via a coupling of two piperazine rings of HL1 on a carbon atom coming from DMF solvent. The dinuclear building units in 1 and 2 are linked into complex supramolecular networks through hydrogen and coordination bondings, resulting in 2D and 1D architectures, respectively. Single-point and broken-symmetry DFT calculations disclosed negligible singlet–triplet splittings within the dinuclear copper fragments in 1 and 2. Catalytic studies showed a remarkable activity of 1 and 2 towards cyclohexane oxidation with H2O2 in the presence of nitric acid and pyridine as promoters and under mild conditions (yield of products up to 21%). Coordination compound 1 also acts as an active catalyst in the intermolecular coupling of cyclohexane with benzamide using di-tert-butyl peroxide (tBuOOtBu) as a terminal oxidant. Conversion of benzamide at 55% was observed after 24 h reaction time. By-product patterns and plausible reaction mechanisms are discussed.

scholarly journals Structural Characterization of Graphene Oxide: Surface Functional Groups and Fractionated Oxidative Debris

Nanomaterials ◽  
2019 ◽  
Vol 9 (8) ◽  
pp. 1180 ◽  
Author(s):  
Elvin Aliyev ◽  
Volkan Filiz ◽  
Muntazim M. Khan ◽  
Young Joo Lee ◽  
Clarissa Abetz ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Graphene Oxide ◽  
Functional Groups ◽  
Structural Model ◽  
Oxide Surface ◽  
Resonance Spectroscopy ◽  
X Ray Diffraction ◽  
Surface Functional Groups ◽  
X Ray ◽  
Transmission Electron

The purpose of this work is the structural analysis of graphene oxide (GO) and by means of a new structural model to answer the questions arising from the Lerf–Klinowski and the Lee structural models. Surface functional groups of GO layers and the oxidative debris (OD) stacked on them were investigated after OD was extracted. Analysis was performed successfully using Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy (UV-Vis), X-ray photoemission spectroscopy (XPS), energy-dispersive X-ray spectroscopy (EDX), Raman spectroscopy, solid-state nuclear magnetic resonance spectroscopy (SSNMR), standardized Boehm potentiometric titration analysis, elemental analysis, X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The analysis showed that graphene oxide layers, as well as oxidative debris contain different functional groups such as phenolic –OH, ketone, lactone, carboxyl, quinone and epoxy. Based on these results, a new structural model for GO layers is proposed, which covers all spectroscopic data and explains the presence of the other oxygen functionalities besides carboxyl, phenolic –OH and epoxy groups.

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