Structure of lithium benzilate hemihydrate solved by simulated annealing and difference Fourier synthesis from powder data

Abstract

The crystal structure of lithium benzilate hemihydrate (C(14)H(11)O(3)(-)Li(+).0.5H(2)O) was solved from synchrotron powder diffraction data. This compound crystallizes in the monoclinic space group P2(1)/a. The structure was solved via the direct space search for two benzilate fragments using the simulated-annealing program DASH, localization of the lithium ions and water molecule from a difference Fourier map, and a restrained Rietveld refinement (R(wp) = 0.0687). The structure is a coordination polymer of [Li(2)(C(14)H(11)O(3))(2).H(2)O](2) tetramers building helical fourfold one-dimensional channels parallel to [010]. Inside the channels the tetrahedral coordination spheres of the lithium ions contain hydroxyl and carbonyl groups, and water molecules. The water molecule functions as the cohesive entity forming extended hydrogen-bonded chains running along [010], and bifurcated donor hydrogen bonds with the two nearest carboxylates. At the outer edge of the channels, weaker intermolecular C-H.Ph hydrogen bonds along [100] and [001] contribute to the supramolecular aggregation of the structure.

Synthesis, Crystal Structure and Hirshfeld Surface Analysis of a New Coordination Polymer: Strontium Benzilate

“…The orientations of the phenyl rings in the benzilate moieties are those of propeller blades, as found in lithium benzilate 13 , potassium benzilate 14 , and the various benzilate derivatives found in the CSD Database 37 . This conformation minimizes the repulsive interactions between the geminal phenyl rings.…”

“…In continuation of our previous investigation on coordination polymers 13,14,[24][25][26][27] , in this work, we present the synthesis, structural characterization and energetic properties of the new coordination polymer strontium benzilate. Hirshfeld surface analysis 28 was used for visually analyzing intermolecular interactions in the crystal structure.…”

Aqua(2-oxido-2,2-diphenylacetato-κ2O1,O2)(1,10-phenanthroline-κ2N,N′)copper(II)

“…In the structural investigations of benzilate complexes, it has been found that the benzilic acid functions as a multidentate ligand with versatile binding and coordination modes (Mora et al, 2003;Rojas et al, 2003). In this paper, we report the structure of the title compound, a copper(II) complex obtained by the reaction of benzilic acid, 1,10-phenanthroline (phen) and copper chloride in an alkaline aqueous solution.…”