Heterogeneous reactions of solid nickel(II) complexes, III
01 Jun 1972-Journal of Thermal Analysis and Calorimetry (Springer Netherlands)-Vol. 4, Iss: 1, pp 61-71
TL;DR: In this article, the stochastic properties of the thermal decomposition of Ni(pyNO)Cl2H2O (I, III, IV, VIII) and Ni(4-MepyNO)2Cl2(V, VI, VII) were studied.
Abstract: The stoichiometry of thermal decomposition was studied for the following compounds: Ni(pyNO)Cl2H2O (I), (pyNO=pyridine N-oxide), Ni(2-MepyNO)Cl2·2H2O (II), Ni(3-MepyNo)Cl2·2H2O (III) and Ni(4-MepyNO)2Cl2·C2H5OH (IV). The heating of the compounds led first to the release of H2O molecules (or C2H5OH molecules), with the formation of Ni(pyNO)Cl2 (V), Ni(2-MepyNO)Cl2(VI), Ni(3-MepyNO)Cl2 (VII) and Ni(4-MepyNO)2Cl2 (VIII). In the next stage, decomposition of the heterocyclic liugands set in. The compositions and spectral and magnetic properties of these complexes indicate their dimeric (II, III, IV, VIII) of polymeric (I, V, VI, VII) structure with coordinated molecules of H2O (or C2H5OH).
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TL;DR: In this paper, the title compound was used for preparation of complexes Cu2(ac)4(bfp)2 (8) and CoCl2(BFp) 2 (9), where ac=CH3CO 2 − 2 − 3 CO 2 and bfp=[1]benzofuro[3,2-c]pyridine.
Abstract: (E)-3-(1-Benzofuran-2-yl)propenoic acid (1) was prepared from 1-benzofuran-2-carbaldehyde under the Doebner’s conditions. The obtained acid was converted to the corresponding azide 2, which was cyclized by heating in diphenyl ether to [1]benzofuro[3,2-c]pyridine-1(2H)-one (3). This compound was aromatized with phosphorus oxychloride to chloroderivative 4 which was reduced with zinc and acetic acid to the title compound 5. [1]Benzofuro[3,2-c]pyridine-2-oxide (6) was synthesized by reaction of 5 with 3-chloroperoxybenzoic acid in dichloromethane. Treatment of 6 with benzoyl chloride and potassium cyanide (Reissert-Henze reaction) was shown to produce the corresponding [1]benzofuro[3,2-c]pyridine-1-carbonitrile (7). The title compound was used for preparation of complexes Cu2(ac)4(bfp)2 (8) and CoCl2(bfp)2 (9), where ac=CH3CO
2
−
and bfp=[1]benzofuro[3,2-c]pyridine. Both oxygen atom of carboxylate ions is used in the coordination to Cu(II). Thermal properties of the complexes 8 and 9 have been studied by TG and DTA and both complexes exhibited high thermal stability while complex 9 are thermally more stable than complex 8.
73 citations
TL;DR: In this article, the metastable zone width and inductions periods of benzophenone in CHCl3 and CCl4 were determined using induction period, and the nucleation parameters, such as the radius of the critical nuclei (r*), the free energy change for the formation of a critical nucleus (ΔG*) and the number of molecules in the critical nucleus were also calculated.
Abstract: Benzophenone is a well-known material, which exhibits non-linear optical (NLO) property. It has been grown by solution technique adopting slow evaporation method from solvents CHCl3, CCl4 for the first time. Solubility metastable zone width and inductions periods of benzophenone in CHCl3 and CCl4 were determined. Interfacial tension values at two different temperatures for various super saturations, such as 1.10, 1.15, 1.20 and 1.25 were determined using induction period. From interfacial tension values, the nucleation parameters, such as the radius of the critical nuclei (r*), the free energy change for the formation of a critical nucleus (ΔG*) and the number of molecules in the critical nucleus were also calculated for benzophenone in CHCl3 and CCl4 at two different temperature. The effect of surface tension, viscosity, density of these solvents are correlated with interfacial tension. The metastable zone width is also correlated with interfacial tension. The solution grown crystals were carefully harvested and subjected to various characterization studies to check its purity and to determine its applicability.
40 citations
TL;DR: Three zinc compounds have been synthesized using DTA-TG, IR spectra and X-ray and the dithiocarbamate and phosphate contents have been determined spectrophotometrically and volumetrically, respectively.
Abstract: Zinc diethyldithiocarbamate, zinc diethyldithiocarbamate-phosphate and zinc phosphate have been synthesized. They have been characterized using DTA-TG, IR spectra and X-ray. The dithiocarbamate and phosphate contents have been determined spectrophotometrically and volumetrically, respectively. Fungicidal activity of the compounds has been tested by well diffusion method using fungi Fusarium sp.
39 citations
TL;DR: In this article, the solid-state thermal dissociation reactions of the complexes of all the lanthanide(III) nitrates and thiocyanates (except Pm) with the cyclic polyether dibenzo-18-crown-6 were investigated.
30 citations
TL;DR: In this article, the stochastic geometry of 2-Rpy has been investigated and it was shown that 2-rpy is square-planar and has pseudo-octahedral geometry.
Abstract: The Stoichiometry of thermal decomposition was studied for the following compounds: Ni(NCS)2(2-Mepy)2 (I), (Me=methyl, py=pyridine), Ni(NCS)2(2-Etpy)2 (II) (Et=ethyl), Ni(NCS)2(2-Clpy)2 (III), Ni(NCS)2(2-Brpy)2 (IV), Ni(NCS)2(2-NH2py)2 (V), Ni((NCS)2(2-NH2py)2·3/4 (C2H5)2O (VI). The release of volatile ligands 2-Rpy is a one-step process for complexes I, II, III and IV, while for V and VI it is a two-step process, Ni(NCS)2(2-NH2py)1 (VII) being formed as an intermediate complex. It was found that complexes I and II are square-planar; the others exhibited pseudo-octahedral geometry. The differences in stereochemistry of the above complexes are explained by the different electronic properties of 2-Rpy.ZusammenfassungDie Stöchiometrie der thermischen Zersetzung folgender Verbindungen wurde untersucht: Ni(NCS)2(2-Mepy)2 (I) (Me=Methyl, py=Pyridin), Ni(NCS)2(2-Etpy)2 (II) (Et=Äthyl), Ni(NCS)2(2-Clpy)2 (III), Ni(NCS)2(2-Brpy)2 (IV), Ni(NCS)2(2-NH2py)2 (V), Ni(NCS)2(2-NH2py)2·3/4 (C2H5)2O (VI). Das Entweichen des flüchtigen Ligands 2-Rpy ist ein einstufiger Vorgang für die Komplexen I, II, III und IV, wogegen es für V und VI ein zweistufiger Vorgang ist, wobei Ni(NCS)2(2-NH2py)1 (VII) sich als intermediärer Komplex bildet. Die Komplexe I und II sind quadratisch; die anderen zeigten eine pseudooktaedrische Geometrie. Die Unterschiede in der Stöchiometrie der obigen Verbindungen werden durch die unterschiedlichen elektronischen Eigenschaften von 2-Rpy erklärt.РезюмеИзучена стехиометри я термического разложения ряда соед инений Ni(NCS)2(2-Rpy)2, где Me=метил - (I), этил- (II), Cl - (III), Вг- (IV) и Ni(NCS)2(2-NH2py)4 (V), а также Ni(NCS)2(2-NH2py)2 · 3/4 (C2H5)2О (VI). Выделение летучих ли гандов - 2-Rpy - является одноступенчатым про цессом в случае комплексов I–IV, и двухст упенчатым — в случае к омплексов V и VI, приводя к образова нию промежуточного соед инения Ni(NCS)2(2-NH2py)1, где во все х случаях ру-пиридин. Найдено, что комплекс ы I и II являются плоским и квадратными, а осталь ные комплексы имеют псевдооктаэдр ическую структуру. Ра зличия в стереохимии изученн ых комплексов обьясняется различн ыми электронными сво йствами лиганда 2-Rpy.
28 citations
References
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Book•
30 Jun 1972TL;DR: An overview of Chemical Reaction Engineering is presented, followed by an introduction to Reactor Design, and a discussion of the Dispersion Model.
Abstract: Partial table of contents: Overview of Chemical Reaction Engineering. HOMOGENEOUS REACTIONS IN IDEAL REACTORS. Introduction to Reactor Design. Design for Single Reactions. Design for Parallel Reactions. Potpourri of Multiple Reactions. NON IDEAL FLOW. Compartment Models. The Dispersion Model. The Tank--in--Series Model. REACTIONS CATALYZED BY SOLIDS. Solid Catalyzed Reactions. The Packed Bed Catalytic Reactor. Deactivating Catalysts. HETEROGENEOUS REACTIONS. Fluid--Fluid Reactions: Kinetics. Fluid--Particle Reactions: Design. BIOCHEMICAL REACTIONS. Enzyme Fermentation. Substrate Limiting Microbial Fermentation. Product Limiting Microbial Fermentation. Appendix. Index.
8,257 citations
Book•
01 Jan 1973
TL;DR: In this article, the transition elements involving metal-metal bonds are defined and an introductory essay is given, along with a discussion of homogeneous catalysis and transition metal chemistry, B L Shaw & N I Tucker.
Abstract: (partial) The lanthanides, T Moeller. Carbonyls, cyanides, isocyanides and nitrosyls, W P Griffith. Compounds of the transitional elements involving metal-metal bonds, D L Kepert. Transition metal, J C Green & M V H Green. Nonstoichiometric compounds. An introductory essay, D J M Bevan. Tungsten bronzes, vanadium bronzes and related compounds, P Hagenmuller. Isopolyanions and Heteropolyanions, D L Kepert. Ionic compounds, G C Allen. Transition metal chemistry, B F G Johnson. Organo-transition metal compounds and related aspects of homogenous catalysis, B L Shaw & N I Tucker.
3,003 citations