Diethyl ether paramagnetic

The preparation of another (also paramagnetic) dinitrogen complex, [(CsHsVTiJjNjjMgCl (31), was subsequently reported from reaction of iso-propylmagnesium chloride and Or)-C5H5)2TiCl2 with N2 in diethyl ether at -60°C (76). The complex shows an i>N N absorption at 1255 cm-1 (1215 cm-1 with 15N2), which is even lower than that for [(C5H )2Ti]2N2 (30). Elemental analyses and vibrational data were said to be consistent with these proposed structures ... 

Our samples were prepared by using a composite rod made of graphite and LajOs. llie materials were mixed with a binder (dextrin), partially dried and pressed into a rod. After annealing at 150 °C, the rod was heated to 1,400 C for 2h. The soot produced by arc vaporization of the rod under helium at 200 Torr was extracted with toluene, and the extract was washed with diethyl ether and dried. The resulting powder was analysed using mass spectrometry and electron paramagnetic resonance (EPR) spectroscopy. 

A unique homoleptic molybdenum thiolate, Mo(//r -dmpt)(dmpt)2 (388), is produced in the reaction of MoCl3(thf)3 with Li(2,6-dimesitylphenylthiolate) in diethyl ether at 0°C. The paramagnetic (/rB = 3.6), pseudo-tetrahedral complex features two monodentate thiolates, the third being bound through sulfur and 7r-arene interactions.893 The investigation of Mo111 and MoIV dithiocarbamates as oil additives and lubricant precursors continues. 

Vanadocene and BSD react in diethyl ether to form a dark brown, oxygen-sensitive paramagnetic complex, Cp2V BSD (77), with a terminal isodiazene ligand (72)17 [Eq. (121)]. Compound 77 is stable to 100°C and can be... 

The pale brown, paramagnetic compounds are moderately air-sensitive and should be stored under a dinitrogen atmosphere. In air, solid samples can be kept without apparent decomposition, but solutions rapidly decompose. All the dicarbonyl complexes are soluble in chlorinated solvents and tetrahydro-furan but only sparingly soluble in acetonitrile, alcohols, diethyl ether, and hydrocarbons. Solution infrared samples prepared in air show an additional peak at 1980 cm due to the formation of Tp WOX(CO) during sample preparation. 

Electron spin resonance (ESR) spectra have been used to detect and characterise some paramagnetic ionic compounds which exist as intermediates. An example is l,l,4,4-tetrakis(trimethyl-silyljbutatriene [662] which can be detected only in anionic or cationic form. The anion is obtained with metallic potassium in diethyl ether at 20 °C, and the cation with aluminium chloride in dichloromethane at — 50 to — 70 °C. 

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