Acta Crystallographica · 1965 · 161 citations · 1 references
Natural SciencesChemistryCrystal StructureInorganic ChemistryStructural BiochemistryCrystal ChemistryCrystallographyMolecular StructureNeutron DiffractionStructure DeterminationX-ray CrystallographyCrystal Structure AnalysisCrystal Structure DeterminationCrystal Structure RefinementCrystal Symmetry DeterminationCrystallographic Symmetry AnalysisHydrogen BondingPowder Neutron DiffractionStructure Solution
The crystal structure of uranyl nitrate hexahydrate has been determined by neutron diffraction. The structure is orthorhombic with a = 13.197 + 0.003, b = 8-035 + 0.002, c = 11.467 + 0-003 /~, space group Cmc21. Intensities of 1136 independent reflections with a 2-0< 105 ° were obt~ned with 2= 1065 A. The structure was solved from the three-dimensional neutron Patterson and Fourier syntheses, and refined by a full-matrix least squares, using a statistical weighting scheme. The final weighted R index was 3.9 Vo. The uranyl group is surrounded equatorially by a near-planar oxygen hexagon of four oxygen atoms from two non-equivalent bidentate nitrate groups and two equivalent water oxygens. In the nitrate groups, the N-O bonds involving coordinated oxygens are 0.03--0.05/~ longer than the N-O bonds involving the non-coordinated oxygen atoms; also the O-N-O angles differ significantly from 120 °. All hydrogens are involved in hydrogen bonding and these may be divided into (a) O (water) O (water) hydrogen bonds of length 268-275 A and (b) weaker O (water)O (nitrate)hydrogen bonds of length 2.93 and 2.99/1,. The water molecules associate into sheets perpendicular to the a axis.
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OR FLS--A FORTRAN CRYSTALLOGRAPHIC LEAST-SQUARES PROGRAM
W. R. Busing, K. O. Martin, H. A. Levy · 1962 · 276 citations · Full text