Cesium hexachloroniobate

Cesium hexachloroniobate(V). A thionyl chloride solution (6 ml.) of niobium(V) chloride (1.5 g.) is added to a solution of cesium chloride (1 g.) in iodine(I) chloride (2 ml.) at room temperature. The reaction vessel, similar to the one described above, is stoppered, and the reaction mixture allowed to stand for 2 hours. The resulting precipitate, most of which forms immediately on mixing of the solutions, is isolated by centrifugation, washed with thionyl chloride (10-ml. portions) to remove all the iodine(I) chloride, and vacuum-dried at room temperature. After isolation, the bright yellow cesium hexachloroniobate(V) must be handled in a dry-box. The 3deld is 1.5 g. (62%). Anal. Calcd. for CsNbCle Cs, 30.32 Nb, 21.17 Cl, 48.50. Found Cs, 30.42 Nb, 21.12 Cl, 48.25. 

The properties of niobium (V) chloride are well known. Cesium hexachloroniobate(V) is a bright yellow, crystalline, moisture-sensitive compound. It is soluble in iodine (I) chloride, less so in iodine (I) chloride-thionyl chloride mixtures, and completely insoluble in thionyl chloride it is very slightly soluble in acetonitrile and nitromethane but insoluble in benzene, carbon disulfide, ethyl acetate, and diethyl... 

The yield of cesium hexachloroniobate(V) may be increased by the use of smaller volumes of iodine (I) chloride however, in such instances, care must be taken to avoid using a large excess of cesium chloride since at less than 25 % ICl, this will itself precipitate. 

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See also in sourсe #XX -- [ , ]

See also in sourсe #XX -- [ , ]

See also in sourсe #XX -- [ , ]

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