II Dihydrate

A sample of 1,10-phenanthroline monohydrate (3.96 g, 20 mmole) in 20 mL ethanol is added to a solution of copper(II) chloride dihydrate (3.40 g, 20 mmole) in 40 mL ethanol. A suspension of a green-blue solid develops immediately. A solution of malonic acid (2.08 g, 20 mmole) in 50 mL ethanol is then slowly introduced into this suspension, which is being stirred magnetically. This 

These copper(II) ternary complexes are generally green-blue solids, stable in air, and fairly soluble in water, methanol, and ethanol. Furthermore, those with dicarboxylates and amino acid residues exhibit a characteristic, strong infrared absorption band around 1600 cm 1 due to the coordinated carboxylate group. The infrared spectra from 4000-200 cm 1 as well as the electronic spectra of these complexes have been recorded and assignments made.5 6 

PREPARATIONS OF tams-DIOXOTETRAKIS(PYRIDINE)-RHENIUM(V) CHLORIDE, [Re02py4]Cl, AND PERCHLOROATE, [ReQ2py4] C104 

A study of the different methods of the preparation of [Re02py4]Cl shows that the same quinquevalent rhenium compound is obtained starting from Re(IV) or Re(V) chloro complex. It is known7 that by boiling a mixture of potassium perrhenate, potassium iodide, and hydrochloric acid, a brown product is obtained which contains rhenium mostly in the 5+ oxidation state, with a little of Re(IV). Isolation of pure K2 [ReCl6] or K2[ReOCls] from the brown 

2K2[ReCl6] + 14py + V402 +7H20 ------ 2[Re02py4]Cl-2H20 

After 2 days, red crystals separate, are filtered under suction and washed twice with a small volume (2 mL) of water. The crystals are powdered and extracted with ethanol. The extract is reduced to a very small volume (almost dry) in air or in a desiccator over fused calcium chloride and filtered under suction. The product, [Re02py4]Cl-2H20, is dried in air. Yields are typically 5.0 g (60% based on the amount of KRe04). (The checker obtained a yield of 34%.) The anhydrous compound is obtained by drying over P4O10. The compound is of moderate purity and can be used for ordinary purposes. It can be crystallized by slow evaporation in air of an aqueous ethanolic solution (50=50) containing traces of pyridine. 

For purification, the crude product is dissolved in 30 ml. of concentrated sulfuric acid. To the vigorously stirred solution 11. of water is slowly added. The recrystallized product is collected by suction filtration and washed thoroughly with small 

The bipyridine complex Fe(bipy)2(CN)2-3H20 can be prepared by using 4.7 g. of 2,2 -bipyridine in place of 6.0 g. of 1,10-phenanthroline. Excess, free 2,2 -bipyridine in the filtrate can be recovered by extraction with either benzene or diethyl ether. 

The crude dicyanobis(2,2,-bipyridine)iron(II) can be purified by dissolving it in 25 ml. of concentrated sulfuric acid and diluting it slowly with 800 ml. of water while stirring. The recrystallized product is collected by suction filtration, washed with small portions of water until free of sulfuric acid, sucked dry, rinsed with acetone, and vacuum-dried at room temperature. The final yield is 3.5 g.f (75%). Anal. Calcd. for [Fe(C10H8N2)2(CN)2]-3H20 C, 55.71 H, 4.68 N, 17.72 H20, 11.4 formula weight, 474.3. Found C, 55.8 H, 4.84 N, 17.9 H20, 11.6 formula weight, 472. 

The dark violet, nonionic compounds possess appreciable dibasic character.e 7 They display various colors in different 

Both complexes are readily oxidized to the corresponding ion(III) compounds by strong oxidants in acid solution. They can be successfully titrated with cerium(IV) sulfate in sulfuric acid.4 The equivalence point is best detected potentiometrically (Pt vs. calomel electrode). 

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Complexes of nickel(ii) with ethylenedithiodiacetate, diethylenetri-thioacetate, and ethylidenetetrathiotetra-acetate have been reported. The structure of ethylenedithiodiacetatonickel(ii) dihydrate has been reported. The potentially terdentate ligand, thiodiethanol, forms both 1 1 and 1 2 complexes with nickel. 

Table 32 Properties of Halochromate(II) Dihydrates and a Diacetic Add Adduct...

Triisobutylaluminum-Bis(N-methylsalicylaldimine)nickel. Ni(mesal)2, m.p. 192 -202, is prepared by reaction of bis(salicylaldehyde)nickel(II) dihydrate with N-methyl-amine.1... 

Battaglia, L. P, Corradi, A. B., Menabue, L., Pellacani, G. C., Prompolini, P. and Saladani, M. (1982). Ternary complexes of copper(II) with A-protected amino acids and A -methlyimidazole. Crystal and molecular structures of bis(A-acetyl-a-alaninato)bis(M-methlyimidazole)copper(II) dihydrate. J. Chem. Soc, Dalton Trans., 781. 

The 1 1 cocrystal of 2-amino-5-nitrothiazole with 4-aminobenzoic acid comprises two constituent molecules associated by a hydrogen-bonded graph set dimer through the carboxylic group across the N/N site of the thiazole [0-H...N, 2.614(3)A N-H...O, 2.991(3)A] [144], 2-Bromo-5-nitrothiazole [145], tetrakis (mefa-acetato)bis[2-(2-thionyl)-amino-5-nitrothiazole]-dirhodium-II-dihydrate [146], and /V-(4-melhoxyben/yl (-/WS-nilro-1,3-thia/ol-2-yl) urea [147] have been studied by X-ray analysis. 

An large number of pyrazines were subjected to X-ray crystallographic analysis. Those in the realm of metal complexes included [/i-2,3,5,6-tetrakis(2-pyridyl)pyrazine]bis[chloroplatinum(II)] bis[trichloro(dimethyl sulfoxide-ir5)platinate(II)] 152 <03AX(E)411>, tetraaqua-1,2,4,5-benzenetetracarboxylato(pyrazine)dicobalt(II) dihydrate <03AX(E)841>, polymeric... 

The X-ray structural analyses of bis(oxamide oximato) nickel(II) dihydrate, Ni(OAOH)2 2H20 and bis(oxamide oximato)nickel(II) monohydrate dimethylformamide. 

The synthesis of a vanadium(II) saccharinate complex, namely, tetraaquabis(l,2-benzisothiazol-3(2H)-one 1, l-dioxidato)vanadium(II) dihydrate that satisfies all of these characteristics and can be stored even in the presence of air for a few weeks, without apparent decomposition, is presented here. However, if it is to be kept for long periods of time, it is better to store it under an inert gas. 

Tetraaquabis(l,2-benzisothiazol-3(2H)-one 1, l-dioxidato)vanadium(II) dihydrate is a compound with a remarkable stability toward air, particularly... 

Ci2Fe3H280l6 Hexakis- i-acetatotri(aqua)-p3-oxo-triiron(III,III,II) dihydrate TFXA 307... 

Under air, Ni(N03)2-6H20 (29.8 g, 0.1 mol) and 2,4-pentanedione (20.5 g, 0.205 mol) are dissolved in water (40 mL) and treated with a 0.2 M aqueous solution of NaOH (40 mL). Immediately, a turquoise precipitate is formed. After the addition is complete, the mixture is heated to reflux for 30 min, cooled to ambient temperature, and filtered. The filter cake is washed with water (50 mL) and dried under air for 2 h yield 26.9 g (92%) of light turquoise bis(2,4-pentadionato) nickel(II) dihydrate. In a 500-mL round-bottomed flask attached to a Dean-Stark apparatus, a suspension of bis(2,4-pentadionato)nickel(II) dihydrate (26.9 g,... 

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