Abstract
The tetramethylammonium counterion was used to suppress formation of insoluble uranate salts, M2U2O7, and allow for a detailed structural and spectroscopic characterization of UO2(OH)n2-n (n = 4, 5) under highly alkaline aqueous solution conditions. Single crystals of [Co(NH3)6]2[UO2(OH)4]3·H2O were obtained by cooling a dilute solution of Co(NH3)6Cl3 and UO2(NO3)2·6H2O in 3.5 M (Me4N)OH to 5 °C. The asymmetric unit contains three distinct UO2(OH)42- ions, each displaying a pseudo-octahedral coordination geometry with trans oxo ligands. The three independent UO2(OH)42- ions in the unit cell give average UO and U−OH distances of 1.82(1) and 2.26(2) A, respectively. EXAFS data on solid [Co(NH3)6]2[UO2(OH)4]3·H2O and aqueous UO22+ in 3.5 M (Me4N)OH solution were collected at the U LIII edge, and the resulting radial distribution function shows a single asymmetric peak. For the solid and solution, curve fitting reveals two near neighbors. For the crystalline solid, the first shell was fit with two O atoms at ...
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