A Molecular Chain of Four CoII Ions Stabilized by a Tris-Pyridyl/Bis-?-Diketonate Ligand

2009 ◽  
Vol 62 (9) ◽  
pp. 1130 ◽  
Author(s):  
Leoní A. Barrios ◽  
David Aguilà ◽  
Olivier Roubeau ◽  
Keith S. Murray ◽  
Guillem Aromí

The synthesis and characterization of a tris-pyridyl/bis-β-diketone molecule (H2L) is reported. This compound acts as a hexadentate ligand towards CoII to facilitate the assembly of a tetranuclear molecular chain of closely spaced metals with formula [Co4L2(MeOH)8](NO3)4 (1), which exhibits a very flat [Co4L2]4+ platform, as determined by single-crystal X-ray diffraction crystallography. Complex 1 readily exchanges axial methanol ligands with water molecules. The bulk magnetization of the resulting hydrate, 1a, shows that the metals in the [Co4L2]4+ moiety exhibit spin-orbit coupling and antiferromagnetic exchange interactions.

2020 ◽  
Vol 76 (4) ◽  
pp. 322-327
Author(s):  
Emmanuel Blas Patricio-Rangel ◽  
Margarita Tlahuextl ◽  
Hugo Tlahuext ◽  
Antonio Rafael Tapia-Benavides

The synthesis and characterization of two new 1,3,5-triazines containing 2-(aminomethyl)-1H-benzimidazole hydrochloride as a substituent are reported, namely, 2-{[(4,6-dichloro-1,3,5-triazin-2-yl)amino]methyl}-1H-benzimidazol-3-ium chloride, C11H9Cl2N6 +·Cl− (1), and bis(2,2′-{[(6-chloro-1,3,5-triazine-2,4-diyl)bis(azanediyl)]bis(methylene)}bis(1H-benzimidazol-3-ium)) tetrachloride heptahydrate, 2C19H18ClN9 2+·4Cl−·7H2O (2). Both salts were characterized using single-crystal X-ray diffraction analysis and IR spectroscopy. Moreover, the NMR (1H and 13C) spectra of 1 were obtained. Salts 1 and 2 have triclinic symmetry (space group P-1) and their supramolecular structures are stabilized by hydrogen bonding and offset π–π interactions. In hydrated salt 2, the noncovalent interactions yield pseudo-nanotubes filled with chloride anions and water molecules, which were modelled in the refinement with substitutional and positional disorder.


2014 ◽  
Vol 936 ◽  
pp. 915-918
Author(s):  
Hui Duan Li

A novel zinc organophosphonate was synthesized under solvothermal conditions by using [piperazine-1,4-diyldi (methylene)] bis (phosphonic acid) as a organic ligand. Single-crystal X-ray diffraction analysis reveals that compound 1 crystallized in the triclinic space group P-1 (No. 2). Compound 1 formulated as Zn (O3PCH2NHC4H8NHCH2PO3)·H2O. Compound 1 featured a 3D open-framework. Notably, the structure of compound 1 featured one-dimensional channel in the [00 direction. Water molecules were located in these channels. Further characterizations of compound 1 have been performed, including X-ray powder diffraction, IR, ICP and CHN analyses.


2019 ◽  
Vol 15 (1) ◽  
pp. 30-38
Author(s):  
Darma Santi ◽  
Jacson Victor Morin

Characterization of merbau wood ash (Intsia, spp.) due to the influence of temperature and time of calcination has been studied. The variations in calcination temperature were 500 ᴼC (as M500) and 600 ᴼC (as M600), while the variations in the duration of calcination were 1, 2, and 3 hours, noted as M1, M2, and M3, respectively. Characterization was carried out using X-ray diffraction (XRD) and spectroscopic analysis using FT-IR. XRD results identified the presence of CaCO3 species (rhombohedral structure) and K2Si4O9 species with a hexagonal structure on M500. The M600 species identified Si (cubic structure), SiO2 (cubic structure), K2Si4O9 (hexagonal structure), and CaCO3 (rhombohedral structure). In general, the calcination temperature increases the crystallinity of several compounds contained in merbau wood ash. The length of time calcination reduces the absorption peak due to the decomposition and adsorption reactions of the presence of water molecules bound to the ash material of merbau wood (Intsia, spp).


2018 ◽  
Vol 74 (11) ◽  
pp. 1267-1273
Author(s):  
Shuai He ◽  
Ying Xin ◽  
Jiansheng Li ◽  
Zaiming Zhu ◽  
Peng Zhao ◽  
...  

A novel complex based on the Dawson-like [H3BiW18O60]6−, i.e. (C2H9N2)2[{Cu(C10H8N2)(C2H8N2)}2(H3BiW18O60)]·5.5H2O or (enH)2[{Cu(2,2′-bipy)(en)}2(μ4-H3BiW18O60)]·5.5H2O, (1), where enH is protonated ethane-1,2-diamine, 2,2′-bipy is 2,2′-bipyridine and en is ethane-1,2-diamine, has been synthesized hydrothermally and characterized by elemental analysis, single-crystal X-ray diffraction analysis, IR spectroscopy, powder XRD, and thermogravimetry and differential thermal analysis (TG–DTA). For (1), each [H3BiW18O60]6− anion acts as a tetradentate ligand connecting [Cu(2,2′-bipy)(en)]2+ fragments via two terminal and two bridging O atoms, forming a two-dimensional network structure. Along the a and c axes, polyoxometalate units are arranged in an AB…AB manner. The electrochemical behaviour of (1)–CPE (CPE is a carbon paste electrode) was investigated in 2 M H2SO4 solution by cyclic voltammetry (CV). The redox process of WVI/V takes place at E 1/2 = −0.58 (I–I′) and −0.37 V (II–II′), and at −0.04 V (III–III′) for CuII/0. The magnetic properties of (1) were investigated in the range 2–300 K and indicated the existence of strong antiferromagnetic exchange interactions between the Cu2+ centres.


2000 ◽  
Vol 55 (7) ◽  
pp. 567-575 ◽  
Author(s):  
K. Griesar ◽  
E. A. Soto-Bustamante ◽  
W. Haase

Abstract The syntheses of different nitroxide radicals are reported. The thermal behaviour of the ni­ troxide radicals was examined by polarizing microscopy, differential scanning calorimetry as well as X-ray diffraction experiments. Temperature dependent magnetic susceptibility mea­surements were carried out in order to determine the magnetic properties of these nitroxide radicals. The majority of the radicals presented here show weak antiferromagnetic exchange interactions.


1992 ◽  
Vol 47 (6) ◽  
pp. 829-836 ◽  
Author(s):  
Henry Strasdeit

The isolation of 3,6,9,12-tetraazatetradecane-1,14-diamine (linear isomer of pentaethylenehexamine, linpen) from a technical polyamine mixture is described. In methanol, linpen acts as a hexadentate ligand towards cadmium(II). The solid compounds [Cd(linpen)](BPh4)2 (1), [Cd(linpen)](BPh4)2•2 DMSO (2) and [Cd(linpen)](BF4)2 (3) have been isolated and characterized by elemental analysis, spectroscopy and X-ray powder diffraction. The 113Cd NMR resonance of 1 is at 351 ppm (0.30 M in DMSO-d6, standard: 0.10 M Cd(ClO4)2 in D2O).2 and 3 have been structurally characterized by single-crystal X-ray diffraction. 2: C 2/c; a = 19.337(1)Å, b = 17.937(1)Å, c = 18.584(1)Å, β = 111.54(1)°; Z = 4, R = 0.034, Rw = 0.033.3: P21/n; a = 8.607(1)Å, b = 14.851(2)Å, c = 15.703(2)Å, ß = 91.21(2)°; Z = 4,R = 0.083, Rw = 0.072. Both compounds contain discrete [Cd(linpen)]2+ complexes. The hexamine wraps around the metal ion in a helical manner. This results in a strong distortion of the coordination polyhedron. The mean Cd-N bond lengths are 2.38Å and 2.37Å for 2 and 3, respectively.Models for MN6 centers in metal-polyethyleneimine (PEI) complexes are derived from the structure of [Cd(linpen)]2+. For example, loops at the MN6 site in molecules of linear PEI are proposed.


2014 ◽  
Vol 919-921 ◽  
pp. 2166-2169
Author(s):  
Ya Bing Liu ◽  
Hong Jie Wang ◽  
Hong Kai Zhao

The activated photocatalysts are urgently needed for the application of photocatalytic techniques in environmental pollutant removal. A POM - based photocatalyst with the chemical formula of (4, 4’-H2bpy)( 4, 4’-Hbpy)2[SiW12O40]·4H2O (1) has been hydrothermally synthesized and structurally characterized by the elemental analysis, and single crystal X-ray diffraction. Compound 1 consists of 4, 4’-bipyridine unit and keggin type polyoxometalates [SiW12O40]4-. There are hydrogen-bonding interactions between polyoxometalates, 4, 4’-bipyridine and water molecules in 1, forming a new 3-D networks. The degradation of rhodamine B (RhB) under UV-vis irradiation with 1 as the heterogeneous photocatalyst has been investigated, showing a good photocatalytic property of 1 for RhB degradation.


2011 ◽  
Vol 66 (7) ◽  
pp. 755-758
Author(s):  
Sari M. Närhi ◽  
Janne Asikkala ◽  
Jatta Kostamo ◽  
Marja K. Lajunen ◽  
Raija Oilunkaniemi ◽  
...  

N,N´-Dipropyl-N,N,N´ ,N´-tetramethyl-1,2-ethylenediammonium dichloride (1) and dibromide (2) were prepared by the reaction of N,N,N´,N´-tetramethyl-1,2-ethylenediamine and the corresponding 1-halopropane. The structures of the compounds were characterized by single-crystal X-ray diffraction. 1 · 2H2O crystallizes in the triclinic crystal system, space group P1, with Z = 1, and 2 in the monoclinic crystal system, space group P21/c, with Z = 2. The crystal structures of the salts consist of discrete dications and halide anions. The packing in 1 · 2H2O consists of layers of cations with the chloride anions and water molecules forming hydrogen-bonded chains between the cation layers. In 2, the strongest H· · ·Br hydrogen bonds of 2.8138(6) and 2.8187(7) °A link the cations and anions into doublestranded chains. In both salts, cations and anions are also linked together by a further weak C-H· · ·Cl/Br hydrogen bonding network.


2020 ◽  
Vol 15 (2) ◽  
pp. 62-68
Author(s):  
Viorina Gorinchoy

A new tetra-homonuclear iron(III) cluster, [Fe4O2(Sal)4(H2O)6]·4DMA·0.75H2O, where Sal= salicylic acid and DMA= N,N-dimethylacetamide consolidated via two µ3-oxo- and four salicylate-bridges was synthesized and characterized by IR spectroscopic method as well as by single crystal X-ray diffraction analysis. The structure of the obtained tetranuclear compound consists of four FeIII atoms in a “butterfly” arrangement. The coordination sphere of each of the two central FeIII atoms is generated by two μ3-oxo-bridging atoms and four oxygen atoms provided by the tridentate-bridging Sal2- ligands, while the coordination polyhedron of another two iron atoms involve six oxygen atoms from three water molecules, two salicylic and one μ3-oxigen atom. The Fe-O distances within Fe-O-Fe bridge are of 2.102(3) Å (for wing-body) and 2.038(3) Å (for body-body).


Author(s):  
Kleanthi Sifaki ◽  
Nadiia I. Gumerova ◽  
Gerald Giester ◽  
Annette Rompel

A novel tungstoantimonate, [Na5(H2O)18{(HOCH2)2CHNH3}2][SbVWVI 6O24] (SbW6 ), was synthesized from an aqueous solution and structurally characterized by single-crystal X-ray diffraction, which revealed C2/c symmetry. The structure contains two serinol [(HOCH2)2CHNH3]+ and five Na+ cations, which are octahedrally surrounded by 18 water molecules, and one [SbVWVI 6O24]7− anion. The serinol molecules also play a critical role in the synthesis by acting as a mild buffering agent. Each of the WVI and SbV ions is six-coordinated and displays a distorted octahedral motif. A three-dimensional supramolecular framework is formed via hydrogen-bonding interactions between the tungstoantimonates and cations. Powder X-ray diffraction, elemental analysis, thermogravimetric analysis and IR spectroscopy were performed on SbW6 to prove the purity, to identify the water content and to characterize the vibrational modes of the crystallized phase.


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