Preparation and Characterization of Copper(II) and Nickel(II) Complexes with N-Benzyliminodiacetamide Derivatives

2016 ◽  
Vol 69 (8) ◽  
pp. 896 ◽  
Author(s):  
Neven Smrečki ◽  
Vladimir Stilinović ◽  
Maja Merkaš ◽  
Andrea Lučić ◽  
Boris-Marko Kukovec ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Infrared Spectroscopy ◽  
Aqueous Solutions ◽  
Thermal Analyses ◽  
Crystal Structure Analysis ◽  
Trans Isomers ◽  
X Ray ◽  
Molecular And Crystal Structures

The reactions of substituted N-benzyliminodiacetamides (o-CH3Bnimda, m-CH3Bnimda, p-CH3Bnimda, o-ClBnimda, m-ClBnimda, p-ClBnimda, p-FBnimda, and p-BrBnimda; o-CH3Bn = ortho-methylbenzyl, m-CH3Bn = meta-methylbenzyl, p-CH3Bn = para-methylbenzyl, o-ClBn = ortho-chlorobenzyl, m-ClBn = meta-chlorobenzyl, p-ClBn = para-chlorobenzyl, p-FBn = para-fluorobenzyl, and p-BrBn = para-bromobenzyl) with copper(ii) and nickel(ii) nitrate in aqueous solutions were investigated. Sixteen new complexes [Cu(o-CH3Bnimda)2](NO3)2⋅0.5H2O (1), [Cu(m-CH3Bnimda)2](NO3)2 (2), [Cu(p-CH3Bnimda)2](NO3)2⋅2H2O (3), [Cu(o-ClBnimda)2](NO3)2⋅H2O (4), [Cu(m-ClBnimda)2](NO3)2 (5), [Cu(p-ClBnimda)2](NO3)2⋅2H2O (6), [Cu(p-FBnimda)2](NO3)2⋅2H2O (7), [Cu(p-BrBnimda)2](NO3)2⋅2H2O (8), [Ni(o-CH3Bnimda)2](NO3)2⋅H2O (9), [Ni(m-CH3Bnimda)2](NO3)2⋅2H2O (10), [Ni(p-CH3Bnimda)2](NO3)2⋅H2O (11), [Ni(o-ClBnimda)2](NO3)2 (12), [Ni(m-ClBnimda)2](NO3)2⋅2DMF (13) (DMF = N,N-dimethylformamide), [Ni(p-ClBnimda)2](NO3)2⋅2H2O (14), [Ni(p-FBnimda)2](NO3)2⋅H2O (15), and [Ni(p-BrBnimda)2](NO3)2⋅2H2O (16) were prepared and characterized by infrared spectroscopy and thermal analysis (thermogravimetric and differential thermal analyses). The molecular and crystal structures of three complexes (2, 5, and 13) were determined by X-ray crystal structure analysis. The octahedral coordination environments around the copper(ii) and nickel(ii) ions in complexes 2, 5, and 13 consist of two O,N,O'-tridentate iminodiacetamide ligands. The complexes are trans-isomers with fac-configuration of the chelators.

scholarly journals Synthesis and Characterization of the New Dicyanamide LiCs2[N(CN)2]3

Inorganics ◽  
2018 ◽  
Vol 6 (4) ◽  
pp. 108 ◽  
Author(s):  
Markus Mann ◽  
Olaf Reckeweg ◽  
Richard Dronskowski
Keyword(s):  
Crystal Structure ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Title Compound ◽  
Crystal Structure Analysis ◽  
Synthesis And Characterization ◽  
X Ray ◽  
Ir And Raman ◽  
Single Crystal Structure Analysis

Crystals of LiCs2[N(CN)2]3 were obtained from the reaction of stoichiometric amounts of aqueous solutions of LiCl and CsBr with Ag[N(CN)2]. X-ray single-crystal structure analysis showed that LiCs2[N(CN)2]3 crystallizes isotypically to NaCs2[N(CN)2]3 and adopts the hexagonal space group P63/m (No. 176), with a = 6.8480(8), c = 14.1665(17) Å, and Z = 2. The IR and Raman spectra of the title compound exhibit modes typical for the dicyanamide anion.

Characterization of Three 'Active' Rhodium(III) Hydroxides

1995 ◽  
Vol 48 (3) ◽  
pp. 557 ◽  
Author(s):  
SJ Crimp ◽  
L Spiccia
Keyword(s):  
Thermal Analysis ◽  
Thermal Decomposition ◽  
Infrared Spectroscopy ◽  
Ion Exchange ◽  
Ion Exchange Chromatography ◽  
Exchange Chromatography ◽  
X Ray Diffraction ◽  
X Ray

Pure solutions of [ Rh (H2O)6]3+, dimer [Rh2(μ-OH)2(H2O)8]4+ and trimer [Rh3(μ-OH)4(H2O)10]5+ have been converted into their respective 'active' hydroxides by dropwise addition to an imidazole solution. These 'active' hydroxides have been analysed by a variety of techniques including rhodium determination, infrared spectroscopy, thermal analysis and powder X-ray diffraction. Purity determinations using ion-exchange chromatography showed that the three hydroxides consist primarily of the neutral forms of the starting aqua ion (>96%) with small amounts of species with higher nuclearity. Rhodium analysis and thermogravimetric measurements confirmed the composition of these hydroxides to be Rh (OH)3(H2O)3.H2O, Rh2(μ-OH)2(OH)4(H2O)4 and Rh3(μ-OH)4(OH)5(H2O)5.5H2O. A scheme for the thermal decomposition of each of the hydroxides has been proposed on the basis of the t.g . and d.t.a . data and the knowledge that the final product in each case is α-Rh2O3. Heating of the hydroxides in air resulted in oxidation of RhIII to RhIV (temperature 250-300°C) forming RhO2 which on further heating decomposed to α-Rh2O3 and dioxygen.

Electrochemistry of Oxygenation Catalysts, Part 6 Electrosynthesis, Structure, Analytical and Electrochemical Properties of Monomeric [CoIII(salen)(DMF)2]+ X- Salts (X = PF6, ClO4)

1996 ◽  
Vol 51 (3) ◽  
pp. 388-398 ◽  
Author(s):  
Bernhard Gollas ◽  
Bernd Speiser ◽  
Hartmut Stahl ◽  
Jürgen Sieglen ◽  
Joachim Strähle
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Cyclic Voltammetry ◽  
Crystal Structure Analysis ◽  
Air Oxidation ◽  
Oxidation Of Co ◽  
X Ray ◽  
Reversible Electron Transfer ◽  
Monomeric Structure ◽  
C Nmr

Abstract[CoIII(salen)(DMF)2]+ X- salts [X = PF6, ClO4; salen = bis(salicyliden)ethylendiiminato; DMF = dimethylformamide] have been synthesized by electrochemical and chemical (air) oxidation of CoII(salen). Their monomeric structure with two DMF molecules in the axial positions in both the solid state and DMF solution is shown by X-ray crystal structure analysis, thermal analysis, mass spectroscopy, and 1H and 13C NMR spectroscopy. The electrochemical reduction of the [CoIII(salen)(DMF)2]+ cation is investigated by cyclic voltammetry and com­ pared to the oxidation of the neutral CoII(salen). The redox reaction connecting the cobalt(II) and the cobalt(III) species appears to be a quasi-reversible electron transfer. These properties make the [CoIII(salen)(DMF)2]+ X-salts starting materials for the analysis of the interaction of basic substrates with cobalt(III) species in the context of the biomimetic oxygenation reactions catalyzed by such complexes.

Hydrothermal Synthesis and Structure Characterization of a Bi-Capped Keggin Heteropoly Molybdovanadated Derivative

2014 ◽  
Vol 1004-1005 ◽  
pp. 542-545
Author(s):  
Ya Bing Liu ◽  
Li Guang Xiao
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Building Blocks ◽  
Crystal Structure Analysis ◽  
Structure Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Supramolecular Networks

A new bi-capped Keggin heteropoly molybdovanadated derivative, [Co (en)3]2[SiMo8V6O42]∙6H2O (1) (en = ethylendiamine) has been hydrothermally synthesized and structurally characterized by the elemental analysis, IR, XPS and single crystal X-ray diffraction. The crystal structure analysis reveals that compound 1 consists of [Co (en)3]2+transition metal coordination fragment and the [SiMo8V6O42]4-building blocks, which are linked together via hydrogen-bonding interactions to form a new 3-D supramolecular networks.

scholarly journals Einkristallzüchtung und Röntgenstrukturanalyse des polymeren 1:1-Komplexes zwischen CuCl2 und Pyridazin / Crystal Growth in Gels and X-Ray Characterization of the Polymeric 1:1-Complex of CuCl2 with Pyridazine

1990 ◽  
Vol 45 (2) ◽  
pp. 199-202 ◽  
Author(s):  
Th. Fetzer ◽  
A. Lentz ◽  
T. Debaerdemaeker ◽  
O. Abou-El-Wafa
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Crystal Growth ◽  
Single Crystals ◽  
Crystal Structure Analysis ◽  
Van Der Waals Interactions ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray

Single crystals of Cu(pdz)Cl2 were grown by using gel methods with tetramethoxysilane as the gel-forming reagent. Thermal decomposition is interpreted. Crystal data for the complex : monoclinic, space group C2/c with a = 938.3(3) pm, b = 1242.9(3) pm, c = 675.7(4) pm, β = 128.48(5)°. A crystal structure analysis reveals CuCl2 molecules connected by pyridazine in the form of zigzag-chains. Between these chains there are only Van-der-Waals-Interactions.

The new P-chalcopyrite compound Cu2FeIn2Se5; synthesis, thermal analysis (DTA), and crystal structure analysis by X-ray powder diffraction (XRPD)

2021 ◽  
Vol 67 (1 Jan-Feb) ◽  
pp. 18
Author(s):  
G. E. Delgado ◽  
P. Grima-Gallardo ◽  
J. A. Aitken ◽  
A. Cárdenas ◽  
I. Brito
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Three Dimensional ◽  
Crystal Structure Analysis ◽  
Chalcopyrite Structure ◽  
Distribution Analysis ◽  
X Ray Diffraction ◽  
Quaternary Compound ◽  
X Ray ◽  
Cell Parameters

The Cu2FeIn2Se5 alloy, belonging to the system (CuInSe2)1-x(FeSe)x with x= ⅓, was synthesized by the melt and annealing technique. The differential thermal analysis (DTA) indicates that this compound melts at 1017 K. The crystal structure of this new quaternary compound was established using powder X-ray diffraction. Cation distribution analysis indicates that this material crystallizes in a P-chalcopyrite structure, space group P2c (Nº 112), with unit cell parameters a = 6.1852(2) Å, c = 12.3633(9) Å, V = 472.98(4) Å3. Cu2FeIn2Se5 is a new adamantane type compound derivative of the sphalerite structure, and consists of a three-dimensional arrangement of distorted CuSe4, FeSe4, and InSe4 tetrahedral connected by common faces.

Generation and Structural Characterization of an [(Imidazol-2-ylidene)HfCl5]-Anion/Imidazolium Cation Salt

2003 ◽  
Vol 58 (10) ◽  
pp. 1005-1008 ◽  
Author(s):  
Martin Niehues ◽  
Gerald Kehr ◽  
Roland Fröhlich ◽  
Gerhard Erker
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Structural Characterization ◽  
Crystal Structure Analysis ◽  
Chloride Anion ◽  
Imidazolium Cation ◽  
X Ray ◽  
Hafnium Tetrachloride

The reaction of 1,3-diisopropylimidazolium chloride (3) with benzylpotassium in d5-bromobenzene generates the stable carbene 1,3-diisopropylimidazol-2-ylidene that is trapped by hafnium tetrachloride. A chloride anion is subsequently added to the Hf atom of the resulting intermediate to yield the salt [(1,3-diisopropylimidazol-2-ylidene)HfCl₅−][1,3-diisopropylimidazolium+] 6 that was characterized by an X-ray crystal structure analysis.

scholarly journals Synthesis, Crystal Structure and Spectral Properties of Copper(II) 2-Chloronicotinato Complexes with N-Heterocyclic Ligands

2016 ◽  
Vol 15 (2) ◽  
pp. 190-199 ◽  
Author(s):  
Jozef Miklovič ◽  
Dušan Valigura ◽  
Ingrid Svoboda ◽  
Ján Moncol ◽  
Milan Mazúr
Keyword(s):  
Crystal Structure ◽  
Spectral Properties ◽  
Crystal Structure Analysis ◽  
Synthesis And Characterization ◽  
Epr Spectrum ◽  
Heterocyclic Ligands ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Good Agreement

Abstract The synthesis and characterization of nine new copper(II) complexes [Cu(2-Clnic)2L2] (where 2-Clnic is 2-chloronicotinate anion, L is imidazole – Im, benzimidazole – Bim, furo[3,2-c]pyridine – FP, 2-methylfuro[3,2-c]pyridine – MFP, or [1]benzofuro[3,2-c]pyridine – BFP), [Cu(2-Clnic)2(INA)] (where INA is isonicotinamide), [Cu(2-Clnic)2(4-py)]·H2O (where 4-py is 4-methylpyridine) and [Cu2(2-Clnic)4(IQ)2] (where IQ is isoquinoline) are reported. The characterizations were based on elemental analysis, infrared, electronic and EPR spectra. The dimeric character of [Cu2(2-Clnic)4(IQ)2] is assumed on the EPR spectrum and the other spectral methods. The crystal structure of the [Cu(2-Clnic)2(Bim)2] and [Cu(2-Clnic)2(FP)2] complexes have been determined by X-ray crystal structure analysis. Both complexes exhibit the hexacoordination coordination polyhedra around copper atom that lies in the crystallographic center of symmetry. The distorted tetragonal-bipyramidal (4+2) arrangement is in good agreement with spectral data that have suggested an asymmetric chelate coordination of the carboxylic group.

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