Single crystals of two new salt-inclusion uranium(VI) silicates, [NaK 6 F][(UO 2 ) 3 (Si 2 O 7 ) 2 ] and [KK 6 Cl][(UO 2 ) 3 (Si 2 O 7 ) 2 ], were grown from mixed alkali halide salt fluxes. Both compounds crystallize in the [NaRb 6 F][(UO 2 ) 3 (Si 2 O 7 ) 2 ] structure type in the orthorhombic space group Pnnm with lattice parameters a = 11.0819(5) Å, b = 13.1149(6) Å, and c = 7.8418(4) Å ([NaK 6 F]) and a = 11.0830(7) Å, b = 13.5850(4) Å, and c = 7.8693(5) Å ([KK 6 Cl]). The surface area to volume (sa/vol) ratio of the reaction, controlled by the reaction vessel dimensions, has a strong influence on the reaction products with small sa/vol ratios favoring the growth of the salt-inclusion phases. Both compounds exhibit the typical luminescence of the uranyl group with the luminescence of [KK 6 Cl][(UO 2 ) 3 (Si 2 O 7 ) 2 ] being less intense than [NaK 6 F][(UO 2 ) 3 (Si 2 O 7 ) 2 ], likely due to quenching by the Cl − ions.