Isolation and characterization of a tetranuclear Pt–Fe⋯Fe–Pt intermediate en route to the trinuclear Pt–Fe–Pt cluster

2017 ◽  
Vol 46 (40) ◽  
pp. 14012-14020
Author(s):  
Kazuhiro Uemura ◽  
Masahiro Taoka
Keyword(s):  
Single Crystal ◽  
Intermediate Compound ◽  
Mononuclear Complex ◽  
Synthetic Process ◽  
X Ray ◽  
Pt Complex ◽  
Isolation And Characterization ◽  
Physical Measurements ◽  
Pt Cluster

An intermediate compound of a tetranuclear Pt–Fe⋯Fe–Pt complex in the synthetic process to form a trinuclear Pt–Fe–Pt complex by mixing the “amidate-hanging” Pt mononuclear complex and iron sources was successfully isolated and characterized by single-crystal X-ray analysis and several physical measurements.

Isolation and characterization of a novel acid degradation impurity of Amlodipine Besylate using Q-TOF, NMR, IR and single crystal X-ray

2014 ◽  
Vol 99 ◽  
pp. 59-66 ◽  
Author(s):  
Ravi Rapolu ◽  
Ch. Krishnam Raju ◽  
Kolupula Srinivas ◽  
Atul Awasthi ◽  
Sameer G. Navalgund ◽  
...  
Keyword(s):  
Single Crystal ◽  
Amlodipine Besylate ◽  
X Ray ◽  
Acid Degradation ◽  
Isolation And Characterization

scholarly journals Synthesis and crystallographic characterization of N-allyl-N-benzyl-4-methylbenzenesulfonamide

2020 ◽  
Vol 11 (3) ◽  
pp. 245-249
Author(s):  
Brock Anton Stenfors ◽  
Felix Nyuangem Ngassa
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Primary Amine ◽  
X Ray Diffraction ◽  
One Pot ◽  
Synthetic Process ◽  
X Ray ◽  
Cell Parameters

N-Benzyl-4-methylbenzenesulfonamides were prepared via a two-step synthetic process involving the treatment of 4-methylbenzenesulfonyl chloride with a primary amine to give the corresponding 4-methylbenzenesulfonamide. Benzylation of the sulfonamide affords the substituted N-benzyl-4-methylbenzenesulfonamides. The similarities between the two steps of synthesis lend credence to the development of a one-pot synthesis of substituted N-benzyl-4-methylbenzenesulfonamides from 4-methylbenzenesulfonyl chloride. This method was applied to the synthesis of N-allyl-N-benzyl-4-methylbenzenesulfonamide and characterized through spectroscopic and crystallographic means. The crystal structure of N-allyl-N-benzyl-4-methylbenzenesulfonamide was obtained by single-crystal X-ray diffraction. The crystal structure reveals an orthorhombic Pna21 space group with cell parameters a = 18.6919 (18) Å, b = 10.5612 (10) Å, c = 8.1065 (8) Å, V = 1600.3 (3) Å3 and Z = 4, T = 173.15 K, μ(MoKα) = 0.206 mm-1, Dcalc = 1.251 g/cm3, 14455 reflections measured (4.36° ≤ 2Θ ≤ 54.96°), 3619 unique (Rint = 0.0439, Rsigma = 0.0429) which were used in all calculations. The final R1 was 0.0428 (I > 2σ(I)) and wR2 was 0.1079 (all data). Molecules are linked through C-H···N hydrogen bonds and C-H···π interactions.

A portable light-delivery device forin situphotocrystallographic experiments in the home laboratory

2016 ◽  
Vol 49 (4) ◽  
pp. 1383-1387 ◽  
Author(s):  
Radosław Kamiński ◽  
Katarzyna N. Jarzembska ◽  
Sylwia E. Kutyła ◽  
Marek Kamiński
Keyword(s):  
Single Crystal ◽  
Structural Changes ◽  
Delivery Device ◽  
X Ray ◽  
Light Delivery ◽  
Isolation And Characterization ◽  
Laser Focusing ◽  
Additional Sample

Photocrystallographic experiments provide valuable information on how crystalline samples interact with light, yielding light-induced structural changes. Studied processes include, among others, solid state chemical reactions, as well as isolation and characterization of various metastable states. Thus, some instrumentation development efforts in the field have been dedicated to facilitating such experiments using a home X-ray source. In this contribution, a portable, easy-to-use and adjustable light-delivery device for home single-crystal diffractometers is described. The whole system consists of adjustable laser-focusing optics and a holder, which can be conveniently attached to a goniometer, as an additional sample conditioning device. The light-delivery device was designed to reduce any goniometer movement limitations. It allows one to conveniently perform photocrystallographic experiments without violation of the X-ray safety protocols, even when changing the light source is necessary. Testin situphotocrystallographic experiments performed on the literature-reported Ni(NO2)2(dppe) complex [dppe is bis(diphenylphosphino)ethane] confirm the effectiveness and applicability of the device for conducting linkage isomer single-crystal-to-single-crystal transformations.

Spin-crossover iron(II) long-chain complex with slow spin equilibrium at low temperature

2021 ◽  
Author(s):  
Qi Zhao ◽  
Jin-Peng Xue ◽  
Zhi-Kun Liu ◽  
Zi-Shuo Yao ◽  
Jun Tao
Keyword(s):  
Low Temperature ◽  
Single Crystal ◽  
Spin Crossover ◽  
Chain Complex ◽  
Mononuclear Complex ◽  
X Ray ◽  
Alkyl Chains ◽  
Long Chain

A mononuclear complex with long alkyl chains, [FeII(H2Bpz2)2(C9bpy)] (1; H2Bpz2 = dihydrobis(1-pyrazolyl)borate, C9bpy = 4,4'-dinonyl-2,2'-bipyridine), was synthesized. Single-crystal X-ray crystallographic studies revealed that - and - forms of the complex...

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.

Electrocrystallizing C60: synthesis, single crystal x-ray structure, and magnetic (ESR, SQUID) characterization of [(C6H5)4P]2[C60][I]x

1993 ◽  
Vol 115 (22) ◽  
pp. 10392-10393 ◽  
Author(s):  
Alain Penicaud ◽  
Aaron Perez-Benitez ◽  
R. Gleason V. ◽  
E. Munoz P. ◽  
R. Escudero
Keyword(s):  
Single Crystal ◽  
X Ray

Structural Systematics of Rare Earth Complexes. VII. Crystal Structure of Bis(2,2'/6',2␛-Terpyridinium) Octaaquaterbium(III) Heptachloride Hydrate

1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Rare Earth ◽  
Single Crystal ◽  
Structural Characterization ◽  
Title Compound ◽  
Room Temperature ◽  
Chloride Ions ◽  
Full Matrix ◽  
X Ray

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.

scholarly journals After 200 Years: The Structure of Bleach and Characterization of Hypohalite Ions by Single‐Crystal X‐Ray Diffraction

2021 ◽  
Author(s):  
Filip Topić ◽  
Joseph M. Marrett ◽  
Tristan H. Borchers ◽  
Hatem M. Titi ◽  
Christopher J. Barrett ◽  
...  
Keyword(s):  
Single Crystal ◽  
X Ray Diffraction ◽  
X Ray

Isolation and characterization of lignocellulosic fiber from jute bast by the organic solvent degumming system: an alkali-free method

2021 ◽  
pp. 004051752110154
Author(s):  
Zhihui Qin ◽  
Shuyuan Zhao ◽  
Liu Liu ◽  
Zhaohe Shi ◽  
Longdi Cheng ◽  
...  
Keyword(s):  
National Standards ◽  
X Ray Diffraction ◽  
High Concentration ◽  
X Ray ◽  
Lignocellulosic Fibers ◽  
Lignocellulosic Fiber ◽  
Isolation And Characterization ◽  
Alkali Consumption ◽  
Scanning Electron

Degumming is the dominant method for insolating lignocellulosic fibers in textile applications. Traditional alkaline degumming (TAL), as a common method, requires a high-concentration alkali and has been a severe challenge to the environment. In the research reported here, the possibility of innovative jute degumming by organic solvents 1-2 propylene glycol and a combination of additive green oxygen (GO-OS) was studied. The results revealed that fibers could be extracted by this system (under condition of 0.9% GO-OS, 180°C, 120 min), and obtained fibers with higher breaking tenacity (7.1 cN/dtex), yield (65.7%), breaking elongation (2.87%) and residual gum (11.7%), which all meet the requirement of the relevant Chinese Textile National Standards. Notably, the required reaction time (120 min) of the GO-OS system was 180 min shorter than that of the TAL method. Furthermore, the modifications introduced by the degumming effect on physicochemical aspects were characterized and confirmed by Fourier transform infrared spectroscopy, scanning electron microscopy and X-ray diffraction. This study provides a promising degumming method for separating jute lignocellulose without acid and alkali consumption.

scholarly journals Arene Ruthenium Metalla-Assemblies with Anthracene Moieties for PDT Applications

Inorganics ◽  
2018 ◽  
Vol 6 (3) ◽  
pp. 97 ◽  
Author(s):  
Marie Gaschard ◽  
Farzaneh Nehzat ◽  
Thomas Cheminel ◽  
Bruno Therrien
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
General Formula ◽  
Structure Analysis ◽  
White Light ◽  
Light Irradiation ◽  
Synthesis And Characterization ◽  
X Ray

The synthesis and characterization of three metalla-rectangles of the general formula [Ru4(η6-p-cymene)4(μ4-clip)2(μ2-Lanthr)2][CF3SO3]4 (Lanthr: 9,10-bis(3,3’-ethynylpyridyl) anthracene; clip = oxa: oxalato; dobq: 2,5-dioxido-1,4-benzoquinonato; donq: 5,8-dioxido-1,4-naphthoquinonato) are presented. The molecular structure of the metalla-rectangle [Ru4(η6-p-cymene)4(μ4-oxa)2(μ2-Lanthr)2]4+ has been confirmed by the single-crystal X-ray structure analysis of [Ru4(η6-p-cymene)4(μ4-oxa)2(μ2-Lanthr)2][CF3SO3]4 · 4 acetone (A2 · 4 acetone), thus showing the anthracene moieties to be available for reaction with oxygen. While the formation of the endoperoxide form of Lanthr was observed in solution upon white light irradiation, the same reaction does not occur when Lanthr is part of the metalla-assemblies.

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