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Two new Tl uranyl compounds, Tl 2 (UO 2 )(MoO 4 ) 2  and Tl 2 (UO 2 )(CrO 4 ) 2 , have been prepared by high-temperature solid-state reaction and hydrothermal synthesis, respectively. The structure of Tl 2 (UO 2 )(MoO 4 ) 2  (orthorhombic,  Pca 2 1 ,  a  = 10.977(3),  b  = 14.004(3),  c  = 14.041(3) Å,  V  = 2158.5(8) Å 3 ,  Z  = 8) has been solved by direct methods and refined to  R  1  = 0.051 on the basis of 5229 unique observed reflections (| F  o | ≥ 4 σ  F ). The structure of Tl 2 (UO 2 )(CrO 4 ) 2  (orthorhombic,  Pca 2 1 ,  a  = 10.7034(5),  b  = 13.4252(6),  c  = 13.9364(6) Å,  V  = 2002.6(2) Å 3 ,  Z  = 8) has been solved by direct methods and refined to  R  1  = 0.035 on the basis of 6330 unique observed reflections (| F  o | ≥ 4 σ  F ). The compounds are isostructural and are based upon [(UO 2 )( A O 4 ) 2 ] sheets ( A  = Cr, Mo) of  Ur O 5  pentagonal bipyramids ( Ur  = UO 2  2+ , uranyl ion) that share equatorial corners with  A O 4  tetrahedra. The sheets are parallel to (001) and are linked by Tl +  cations located in the interlayer. Stereoactive lone electron pairs on the Tl +  cations form lone pair-containing cavities that form channels parallel to the  a  axis and are located at the level of  y  ∼ 0.5. The repulsion of the Tl +  cations across the cavities leads to the distortion of the cation arrangements and, as a consequence, distortion of the flexible [(UO 2 )( A O 4 ) 2 ] uranyl molybdate/chromate sheets.

zeitschrift für kristallographie - crystalline materials

Lone electron pair stereoactivity, cation arrangements and distortion of heteropolyhedral sheets in the structures of Tl 2 [(UO 2 )( A O 4 ) 2 ] ( A  = Cr, Mo)