Coordination polymer of uranyl nitrate with 4,4,10,10-Tetramethyl-1,3,7,9-Tetraazaspiro[5.5]undecane-2,8-dione (Spirocarbone, Sk): Synthesis and study of molecular and crystal structures

Abstract

The coordination polymer {[UO2(NO3)2(C11H20N4O2)] · 2H2O}n (I) was obtained and examined by X-ray diffraction. The crystals are monoclinic, space group C2/c; a = 23.1386(13), b = 5.41575(15), c = 19.7769(11) A, β = 125.285(8)°, V = 2023.01(17) A3, ρcalcd = 2.20 g/cm3, Z = 4. The U atom occupies a special position in the center of inversion. Its coordination polyhedron is a distorted hexagonal bipyramid with axial oxo ligands. In the equatorial plane, the U(1) atom is coordinated by four O atoms of two bidentate nitrate anions and two O atoms of two carbonyl groups of organic spirocarbone (Sk) molecules, which are related by the symmetry operation (0.5 − x, 0.5 − y, −z). In the crystal, polymer chains are parallel to the direction (101). Water molecules are hydrogen-bonded to the N(1) atom of ligand Sk; in addition, they are linked together by the intermolecular hydrogen bonds O(6)-H(6d)…O(6)i(i1/2 − x, −1/2 + y, 1/2 − z); H…O 2.11 A angle O-H…O 160°) and to the nitrate anions by the hydrogen bonds O(6)-H(6e)…O(3)i; H…O 2.29 A; the angle O-H…O 149°). In the crystal, hydrogen-bonded water molecules form chains along the axis y that are perpendicular to the coordination polymers. To verify the purity of complex I, the Rietveld refinement of its X-ray powder diffraction pattern was performed. At room temperature, the unit cell parameters are a = 23.2965(6), b = 5.51225(15), c = 19.8588(6) A, β = 125.6063(17)°, V = 2073.40(10) A3.