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The complexes 4[ UO,( 0,) (CO,)]*H,O (A = Na or K) have been synthesised from the reaction of the product obtained by treating UO,( N0,),*6H20 with AOH and AHCO, (ratio U : Cot-= 1 : 4) with an excess of 30% H,O, at pH 7-8, and A,[VO(0,),(C0,)]~3H20 (A = Na or K) have been synthesised by treating V, O, with A,CO, (ratio V: C o t -= 1 : 1.5) and an excess of 30% H, O, at pH ca. 7. They were precipitated with ethanol. The occurrence of trans O=U=O and terminal V=O in the [UO,(O,) (CO3)I2and [VO(02)2(C03)]3ions, respectively, and the presence of triangular bidentate OZ2and chelated bidentate C o tgroups, have been ascertained from i.r. and laser Raman spectra. The complexes A,[UO,(O,) (CO,) ]-H,O can be dehydrated at ca. 100 "C, a temperature at which A3[VO(02),(C03)]~3H20 starts to decompose.

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