Reinholdt, Marc, Croissant, Jonas, Di Carlo, Lidia, Granier, Dominique, Gaveau, Philippe, Bégu, Sylvie, Devoisselle, Jean-Marie, Mutin, P. Hubert, Smith, Mark E., Bonhomme, Christian, Gervais, Christel, Lee, Arie van der and Laurencin, Danielle. (2011) Synthesis and characterization of crystalline structures based on phenylboronate ligands bound to alkaline earth cations. Inorganic Chemistry, Vol.50 (No.16). pp. 7802-7810. ISSN 0020-1669

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Abstract

We describe the preparation of the first crystalline compounds based on arylboronate ligands PhB(OH)(3)(-) coordinated to metal cations: [Ca(PhB(OH)(3))(2)], [Sr(PhB(OH)(3))(2)]center dot H(2)O, and [Ba(PhB(OH)(3))(2)]. The calcium and strontium structures were solved using powder and single-crystal X-ray diffraction, respectively. In both cases, the structures are composed of chains of cations connected through phenylboronate ligands, which interact one with each other to form a 2D lamellar structure. The temperature and pH conditions necessary for the formation of phase-pure compounds were investigated: changes in temperature were found to mainly affect the morphology of the crystallites, whereas strong variations in pH were found to affect the formation of pure phases. All three compounds were characterized using a wide range of analytical techniques (TGA, IR, Raman, XRD, and high resolution (1)H, (11)B, and (13)C solid-state NMR), and the different coordination modes of phenylboronate ligands were analyzed. Two different kinds of hydroxyl groups were identified in the structures: those involved in hydrogen bonds, and those that are effectively "free" and not involved in hydrogen bonds of any significant strength. To position precisely the OH protons within the structures, an NMR-crystallography approach was used: the comparison of experimental and calculated NMR parameters (determined using the Gauge Including Projector Augmented Wave method, GIPAW) allowed the most accurate positions to be identified. In the case of the calcium compound, it was found that it is the (43)Ca NMR data that are critical to help identify the best model of the structure.

Item Type:	Journal Article
Subjects:	Q Science > QC Physics Q Science > QD Chemistry
Divisions:	Administration > Vice Chancellor's Office Faculty of Science > Physics
Library of Congress Subject Headings (LCSH):	Complex compounds -- Synthesis, Brillouin zones, Pseudopotential method, Crystallography, Magnetic resonance imaging, X-rays -- Diffraction, Calcium, Strontium
Journal or Publication Title:	Inorganic Chemistry
Publisher:	American Chemical Society
ISSN:	0020-1669
Date:	August 2011
Volume:	Vol.50
Number:	No.16
Page Range:	pp. 7802-7810
Identification Number:	10.1021/ic200961a
Status:	Peer Reviewed
Publication Status:	Published
Funder:	Seventh Framework Programme (European Commission) (FP7), Royal Society (Great Britain)
Grant number:	ERG 239206 (FP7), JP090313 (RS)
URI:	http://wrap.warwick.ac.uk/id/eprint/38555

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