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Single crystals of four new layered uranyl phosphates, including three oxyfluoride-phosphates, were synthesized by molten flux methods using alkali chloride melts, and their structures were determined by single-crystal X-ray diffraction. Cs 11 [(UO 2 ) 12 (PO 4 ) 3 O 13 ] ( 1 ) and Rb 11 [UO 2 ) 12 (PO 4 ) 3 O 12 F 2 ] ( 2 ) contain uranyl phosphate layers exhibiting a new sheet topology that can be related to that of β-U 3 O 8 , while Cs 4.4 K 0.6 [(UO 2 ) 6 O 4 F(PO 4 ) 4 (UO 2 )] ( 3 ) and Rb 4.4 K 0.6 [(UO 2 ) 6 O 4 F(PO 4 ) 4 (UO 2 )] ( 4 ) contain layers of a known isomer of the prominent phosphuranylite topology. The location of the fluorine in structures  2 - 4  is discussed using bond valence sums. First principles calculations were used to explore why a pure oxide structure is obtained for the Cs containing phase ( 1 ) and in contrast an oxyfluoride phase for the Rb containing phase ( 2 ). Ion exchange experiments were performed on  1  and  2  and demonstrate the ability of these structures to exchange approximately half of the parent alkali cation with a target alkali cation in an aqueous concentrated salt solution. Optical measurements were performed on  1  and  2  and the UV-vis and fluorescence spectra show features characteristic of theUO    2    2  +uranyl group.

frontiers in chemistry

Observation of the Same New Sheet Topology in Both the Layered Uranyl Oxide-Phosphate Cs11[(UO2)12(PO4)3O13] and the Layered Uranyl Oxyfluoride-Phosphate Rb11[(UO2)12(PO4)3O12F2] Prepared by Flux Crystal Growth