Conical fragments

The synthesis of the trismethylenemethane iron tricarbonyl complex [(CH2)3C]-Fe(CO)3 was reported by Emerson et al. in 1966 (27). The geometry of this compound in the gas phase was investigated by Almenningen et al. (28) using electron diffraction methods. These authors pointed out some structural peculiarities which were not amenable to a simple explanation, in particular, why the hypothetical planar (CH2)3C radical is distorted when bound to the Fe(CO)3 conical fragment in such a way that the carbon atoms of the CH2 groups are displaced toward — the iron atom (Fig. 9). 

Elian M, Chen MML, Mingos DMP, Hoffmann R (1976) A comparative study of conical fragments. Inorg Chem 15 1148-1155... 

Add 15 g, of chloroacetic acid to 300 ml. of aqueous ammonia solution d, o-88o) contained in a 750 ml. conical flask. (The manipulation of the concentrated ammonia should preferably be carried out in a fume-cupboard, and great care taken to avoid ammonia fumes.) Cork the flask loosely and set aside overnight at room temperature. Now concentrate the solution to about 30 ml. by distillation under reduced pressure. For this purpose, place the solution in a suitable distilling-flask with some fragments of unglazed porcelain, fit a capillary tube to the neck of the flask, and connect the flask through a water-condenser and receiver to a water-pump then heat the flask carefully on a water-bath. Make the concentrated solution up to 40 ml. by the addition of water, filter, and then add 250 ml. of methanol. Cool the solution in ice-water, stir well, and set aside for ca. I hour, when the precipitation of the glycine will be complete. 

Place 20 g. of dry powdered benzoic acid in C, add 15 ml. (25 g., i.e., a 30% excess) of thionyl chloride and some fragments of porcelain, and then clamp the apparatus on a boiling water-bath as shown so that no liquid can collect in the side-arm of C. Heat for one hour (with occasional gentle shaking), by which time the evolution of gas will be complete. Cool the flask C, detach the condenser and fit it to the side-arm for distillation, using a 360° thermometer for the neck of C. To the lower end of the condenser fit a small conical flask G (Fig. 67(B)) by a cork carrying also a calcium chloride tube. 

As the droplets move through the hot source area, they continue to vaporize. The electric field at the liquid surface increases until ions present in the eluent are ejected from the droplet. Ions are sampled through a conical exit aperture in the mass analyzer. The ionization of the analytes takes place by means of direct ion evaporization of the sample ion or by solvent-mediated CI reactions an ion of the electrolyte ejected from a droplet reacts with a sample molecule in the gas phase and generates a sample ion that is mass analyzed. In addition, fragment ions can be observed due to the high temperatures associated with TSP negative ions are also produced by TSP, and negative ion detection is recommended for acidic compounds. 

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