Solids, microcrystalline

The dinuclear complex [Cu2 (Ls)2] has also been synthesized and isolated (217). In tetrahydrofuran (THF) solution, this species is oxidized by air yielding the diamagnetic, dinuclear deep green (phenoxyl)copper(II) complex [Cu2(Ls )2]X2 (X = C1,C104) as microcrystalline solid and H202. Although both compounds have... 

Type B Systems, Some Solid Components The state of the system is a fluid/solid mixture at to- For example, the vessel may have been fdled with solvent and gases, but one or more of the organics, organometallics, ligands, or inorganics are added as an amorphous or microcrystalline solid. 

Bis(dipivaloylmethanido)Ni(II) (supplied by Strem or synthesized according to the procedure reported by Hammond ), Ni(DPM)2 (0.420 g, 1.0 mmol), is dissolved in methanol (60 mL) and HL (0.174 g, 0.75 mmol) added. After 1 h stirring, a gray microcrystalline solid precipitates, NiL(DPM). After filtration, the solid is washed with methanol and dried in air. Yield 0.313 g (88%). 

PPh2CH2Ph] [Ir(COD)Cl2] is a yellow microcrystalline solid. It is very soluble in methanol, but these solutions decompose quickly. It is soluble in dichloromethane and chloroform, less soluble in acetone, and insoluble in diethyl ether. 

The compound is a golden yellow microcrystalline solid. It is stable in air both as a solid and in solution. It is soluble in water, methanol, and acetonitrile and is insoluble in ether and hexanes. The NMR spectrum (CD3CN) shows two singlets at 6 3.56 (24H, [K(Ci2H2406)]) and 5.23 (5H, C5//5). The infared spectrum of the solid (KBr) shows a single band in the cyanide region at 2119 cm ... 

The complex Co3RuCu(CH3CN)(CO)12 is a moderately air stable, purple, microcrystalline solid [mp 170-175 °C (dec)]. It can be stored under N2 for... 

Adrenochrome ethyl ether H ch3 H OC2Hs 70-72 81 Deep red microcrystalline solid... 

The higher decomposition points were obtained when adrenochrome methyl and ethyl ethers were prepared by oxidation of the appropriate catecholamine in methanol with silver oxide. The BOlid aminochromes were then obtained as microcrystalline solids on addition of dry ether and cooling the resultant solution to — 80°. The slightly less pure products were obtained when the oxidation was carried out in acetonitrile. [R. A. Heacock and B. D. Scott, loc. cit. (footnote c )]. 

Triethylamine (0.16 mL, 1.2 mmole) is then added to the solution with stirring. The mixture is allowed to stand at room temperature for 24 h, during which time a microcrystalline solid separated. The product is isolated by filtration, washed with ether, and dried in vacuo. Yield = 0.29 g (62%). 

Synthesis of the complex. In a 50-mL Schlenk flask, N,N-bis(2-mercapto-ethyl)2-methylthioethylamine (0.1 g, 0.47 mmole) is dissolved in methanol (10 mL) and subsequently cooled to 5°C in an ice bath. To the cooled solution, a solution of anhydrous nickel acetate (84 mg, 0.47 mmole) in methanol (10 mL) is added dropwise with rapid stirring. The product, a red-black, microcrystalline solid, forms immediately and is collected by filtration, washed several times with small amounts of methanol, and dried in vacuo. Yield = 160 mg (65%). The product obtained from purified ligand is pure by elemental analysis. If crude ligand is used, the complex may be purified by recrystallization from CH2C12 (minimum volume for dissolution) upon addition of petroleum ether or hexane (five times the volume of CH2C12 used). 

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