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Treatment of [UO 2 (OTf) 2 ] or [UO 2 I 2 (thf) 3 ] with 1 equiv. of CyMe 4 BTBP in anhydrous acetonitrile led to the formation of [UO 2 (CyMe 4 BTBP)(OTf) 2 ]  (1)  and [UO 2 (CyMe 4 BTBP)I 2 ]  (2)  which crystallized as the cationic forms [UO 2 (CyMe 4 BTBP)(py)][OTf] 2  (3)  and [UO 2 I(CyMe 4 BTBP)][I]  (4)  in pyridine and acetonitrile, respectively. These compounds are unique examples of structurally characterized actinide complexes with a BTBP molecule; this ligand adopts a planar conformation in the equatorial plane of the {UO 2 } 2+  ion. In pyridine,  1  is dissociated into [UO 2 (OTf) 2 (py) 3 ] and free CyMe 4 BTBP and the thermodynamic parameters ( K , Δ H , Δ S ) of this equilibrium have been determined by  1 H NMR spectroscopy. The ethoxide derivative [UO 2 (OEt)(CyMe 4 BTBP)][OTf]  (5)  crystallized from a solution of  1  in a mixture of ethanol and acetone under air, and the dinuclear μ-oxo complex [{UO 2 (CyMe 4 BTBP)} 2 (μ-O)][I] 2  (6)  was obtained from [UO 2 I(thf) 2.7 ] and CyMe 4 BTBP. The crystal structures of  6  and of the analogous derivatives [{UO 2 (py) 4 } 2 (μ-O)][I] 2  (7)  and [{UO 2 (TPTZ)(py)} 2 (μ-O)][I 3 ] 2  (8)  exhibit a flexible [{UO 2 }–O–{UO 2 }] 2+  moiety.

First 5f-element complexes with the tetradentate BTBP ligand. Synthesis and crystal structure of uranyl(VI) compounds with CyMe 4 BTBP