A CuII complex with an carbamoylcyanonitrosomethanide ligand formed in situ by the nucleophilic addition of water to dicyanonitrosomethanide: structure, spectral and magnetic properties

2018 ◽  
Vol 74 (5) ◽  
pp. 584-589 ◽  
Author(s):  
Ivan Potočňák ◽  
Oleksandr Bukrynov ◽  
Andrii Kliuikov ◽  
Erik Čižmár ◽  
Svitlana Vitushkina ◽  
...  

The complex (2,2′-biquinoline-κ2 N,N′)(carbamoylcyanonitrosomethanide-κ2 N,O)chloridocopper(II) acetonitrile monosolvate, [Cu(C3H2N3O2)Cl(C18H12N2)]·CH3CN or [Cu(ccnm)Cl(biq)]·acn (acn is acetonitrile, biq is 2,2′-biquinoline and ccnm is carbamoylcyanonitrosomethanide), (I), was prepared as a result of nucleophilic addition of water to the dicyanonitrosomethanide ion in the presence of CuII and biq. IR spectroscopy confirmed the presence of ccnm, biq and acn in (I). The solid-state structure consists of the neutral complex containing ccnm and biq ligands, coordinated to the CuII atom in a bidendate chelating manner, and a chloride ligand, resulting in a distorted tetragonal pyramidal coordination of CuII. The asymmetric unit is supplemented by one molecule of solvated acn which, along with the nitrile group of ccnm, serves as an acceptor in intermolecular hydrogen bonding, creating infinite chains along the b axis. Magnetic measurements revealed a paramagnetic behaviour with a very small Weiss temperature Θ = −0.32 K and high anisotropy of the g tensor (g x = 2.036, g y = 2.120 and g z = 2.205).

2018 ◽  
Vol 233 (12) ◽  
pp. 877-882
Author(s):  
Ivan Potočňák ◽  
Oleksandr Bukrynov ◽  
Andrii Kliuikov ◽  
Erik Čižmár ◽  
Svitlana Vitushkina ◽  
...  

Abstract From the system CuCl2 – pbi – NaN(CN)2−, polymeric [CuCl(μ1,5-dca)(pbi)]n·nH2O (1) complex (dca=dicyanamide, pbi=2-(2-pyridyl)benzimidazole) was isolated and characterized by structure analysis, spectral and magnetic measurements. Infrared spectroscopy confirmed the presence of pbi, dca and water molecules in 1. Its solid-state structure is formed by infinite chains running along the b axis. In the chain, the Cu(II) atom is penta-coordinated by two nitrogen atoms of chelate pbi ligand, by two nitrile nitrogen atoms of bridging μ1,5-dca and by chloride ligand which occupies the apical position of tetragonal pyramid around the Cu(II) atom. Asymmetric unit is supplemented by one molecule of solvated water, which along with chlorine atom serves as acceptors in intermolecular hydrogen bonds and along with π–π interactions create a 3D supramolecular structure. Magnetic measurements revealed the presence of a weak ferromagnetic exchange interaction J/kB=0.11 K.


Synthesis ◽  
2020 ◽  
Author(s):  
Ikyon Kim ◽  
Sung June Kim ◽  
Sunhee Lee

AbstractBroadening of nitrogen-fused heteroaromatic chemical space such as indolizine and pyrrolo[1,2-a]pyrazine was achieved via FeCl­3-catalyzed nucleophilic addition of these N-fused aromatic compounds to a wide range of azolinium systems generated in situ, leading to novel N-fused heteroaromatic scaffolds with dearomatized N-heterocyclic substituents regioselectively. Nucleophilic addition of indolizines and pyrrolo[1,2-a]pyrazines mainly occurred at the C1 position of the isoquinoliniums and at the C4 site of the quinoliniums.


2000 ◽  
Vol 53 (3) ◽  
pp. 225 ◽  
Author(s):  
Zdenek Smékal ◽  
Zdenek Trávnícek ◽  
Jaromír Marek ◽  
Milan Nádvornik

Five new complexes of compositions [Cu(1,2-pn)2Fe(CN)5NO]·H2O (1,2-pn = propane-1,2-diamine) and [Cu(L)Fe(CN)5NO]·xH2O (L = tmen (N,N,N′,N′-tetramethylethane-1,2-diamine), x = 0.5; L = trimeen (N,N,N′-trimethylethane-1,2-diamine), x = 1; L = dien (N-(2-aminoethyl)ethane-1,2-diamine), x = 0; L = medpt (N-(3-aminopropyl)-N-methylpropane-1,3-diamine), x = 2) have been isolated from the reaction mixture of Cu(ClO4)2·6H2O (or CuCl2·2H2O), the amine and Na2 [Fe(CN)5NO]·2H2O in water. The complexes have been characterized by infrared and ultraviolet–visible spectroscopies, and magnetic measurements. Single-crystal X-ray structural analysis revealed that the [Cu(1,2-pn)2Fe(CN)5NO]·H2O complex assumes a cyanide-bridged binuclear structure in which iron(II) is six-coordinated by five cyanide ligands and one nitrosyl group (the nitrosyl group lies cis to the bridging cyanide group), while copper(II) is five-coordinated by two propane-1,2-diamine ligands and a bridging cyanide ligand in a distorted tetragonal pyramidal arrangement.


2001 ◽  
Vol 56 (10) ◽  
pp. 1025-1034 ◽  
Author(s):  
Markus Ströbele ◽  
H.-Jtirgen Meyer

The title compounds were prepared through reactions of Li2Nb6Cl16 with the corresponding crown ethers in acetone. All three compounds were obtained as dark brown crystals. Their structures were solved with the means of single-crystal X-ray diffraction.[Li(12-crown-4)2][Li(12-crown-4)(OH2)]2[Nb6Cl18]: space group P21/n, Z =2, a = 1320.4(1), b = 1879.1(1), c = 1321.7(1) pm, ß = 92.515(6)°, R1 = 0.0297 (I>2σ(I)). The crystal structure contains Li+ sandwiched by two 12-crown-4-ethers plus Li+ coordinated by one 12-crown-4- ether and one water molecule.[Li(15-crown-5)2(OH2)]3[Nb6Cl18]: space group R3̅, Z = 3, a = b = 2081.7(1), c = 1991.7(1) pm, R1 = 0.0395 (I > 2σ(I)). In the crystal structure Li+ and one water molecule are sandwiched by two 15-crown-5-ethers.[(18-crown-6)2(O2H5)]3[Nb6Cl18]: space group P1̅, Z = 1 ,a = 1405.1(1), b = 1461.1(2), c = 1492.2(2) pm; α = 98.80(1)°, ß = 98.15(1)°, γ = 97.41(1)°, R1 = 0.0538 (I > 2σ(I)). H5O2+ was found in the structure refinement sandwiched between two 18-crown-6-ethers.All compounds reported contain [Nb6Cl18] clusters with Nb-Nb distances between 299 and 301 pm. The paramagnetic behaviour expected for [Nb6Cl18]3- in all three compounds was confirmed by magnetic measurements.


2020 ◽  
Vol 2020 ◽  
pp. 1-8 ◽  
Author(s):  
Midilane S. Medina ◽  
Alessandra Zenatti ◽  
Marcia T. Escote

This work describes a fast and simple procedure that combines the virtues of the microwave-assisted hydrothermal method with an oxidizing agent to produce Co3O4 nanocubes and nanoplates. We observed that particle morphology and size depend on the synthesis time and oxidizing agent (urea and hydrogen peroxide). The X-ray diffraction results showed that the samples are single phase, with crystallite sizes of approximately 30 nm. A similar crystalline domain is observed in the transmission electronic images. Magnetic measurements revealed the influence of the size and morphology of the particles on the magnetic curves. These measurements on the nanoplate samples revealed a paramagnetic behaviour at higher temperatures, and the presence of a cusp at that temperature was defined as TP. The TP decreases from 36 K to 21 K when the size of the plate particles decreases from ~70 nm to 10 nm. These samples also present weak ferromagnetism below TP, which is attributed to a superparamagnetic blockade state. The nanocube samples have a lower magnetic susceptibility magnitude and weak ferromagnetism behaviour at room temperature. Our results show that this synthesis produces Co3O4 nanoplates and nanocubes with interesting magnetic properties related to their shape and size.


1999 ◽  
Vol 562 ◽  
Author(s):  
G. Renaud ◽  
A. Barbier ◽  
C. Mocuta

ABSTRACTCombined in situ structural and ex situ magnetic studies of the Co/NiO(111) and Ni81Fe19/NiO(111) interfaces are presented. The Co and Permalloy films were grown on NiO(111) single crystals. Structural studies were performed by Grazing Incidence X-ray Scattering during growth. The effect of the temperature of the substrate during deposition was investigated. Under specific growth conditions, almost pure FCC Co and NiFe films can be obtained, with small quantities of twins. Magnetic measurements were performed ex situ by Magneto-Optical Kerr Effect (MOKE). A strong correlation between the magnetic properties and the crystallographic structure of the Co film is evidenced. High coercive fields are measured for all samples. High temperature annealing of the NiFe film leads to an improved crystalline quality, but the interface becomes reactive and diffuse: part of the Fe diffuses into the NiO substrate and forms an interface compound, likely to be the spinel NiFe2O4. We also report an in situ grazing incidence X-ray scattering study of the Ni/MgO(001) interface during its formation at room temperature. In-plane measurements reveal that the interface is sharp and that the epitaxial relationship is complex. Two distinct lattices are found to exist: expanded Ni(001) and Ni(110). The latter exhibits several orientations with respect to the substrate depending on the thickness. The Ni(110) orientations disappear by annealing at high temperature, leaving only the Ni cube/cube orientation. The layer was also almost fully transformed into NiO(001) by high temperature oxidation.


1994 ◽  
Vol 9 (2) ◽  
pp. 372-376 ◽  
Author(s):  
T. Harada ◽  
T. Kuji

In the process of crystallization of amorphous melt-spun Nd15Fe77Bx (x = 6–14) alloys, it was found that the crystallization behavior strongly depended upon the boron content even in the same equilibrium three-phase coexistence range. The Nd2Fe14B phase was crystallized directly from the amorphous state in the amorphous Nd-Fe-B materials with relatively lower boron content (Nd15Fe77B6 and Nd15Fe77B8 alloys). In contrast, the metastable body-centered-cubic (bcc) α-iron phase crystallized from the amorphous state prior to the crystallization of the Nd2Fe14B phase in the amorphous Nd-Fe-B materials with relatively higher boron content (Nd15Fe77B10, Nd15Fe77B12, and Nd15Fe77B14 alloys). The existence of the metastable bcc α-iron phase in the amorphous matrix was confirmed by TEM studies, magnetic measurements, and in situ observation by x-ray diffraction. The formation of the metastable phase stabilized the amorphous state, increasing the crystallization temperature of the Nd2Fe14B phase.


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