Author:
Bhuvanesh Nattamai S. P.,Reibenspies Joseph H.,Zhang Yuegang,Lee Peter L.
Abstract
Micro-powder X-ray diffraction patterns of two compounds, namely 3-bromophenylboronic acid and tris(4-bromophenyl)boroxine, were recorded with microgram quantities of sample using a recently developed method employing nylon loops with synchrotron radiation and an image-plate detector. This method, besides using small amount of samples, offers the advantage of recording the powder pattern in the shortest possible time (less than a minute). The structures of the two compounds have been solved byab initiomethods using real-space techniques (simulated annealing and/or parallel tempering) followed by Rietveld refinements with soft restraints on the bond lengths of the rigid bodies. The former compound crystallizes in the monoclinic system [a= 15.7797 (4),b= 5.3085 (2),c= 9.3757 (3) Å, β = 93.357 (3)°; space groupP21/c;Z= 4;Rp= 16.060,Rwp= 10.543,RB= 4.25] with sheets of individual molecules linked through an extended hydrogen-bonding network. Tris(4-bromophenyl)boroxine, displaying molecular disorder, crystallizes in the orthorhombic system [a= 18.9289 (6),b= 21.8872 (6),c= 4.8842 (2) Å; space groupPnma;Z= 4;Rp= 13.270,Rwp= 12.083,RB= 6.06], with discrete molecules held by weak van der Waals forces in a zigzag fashion. It is believed that this is the first time that powder X-ray diffraction patterns using microgram samples have been successfully employed for the structure solution and refinement of molecules with reasonable complexity.
Publisher
International Union of Crystallography (IUCr)
Subject
General Biochemistry, Genetics and Molecular Biology
Cited by
10 articles.
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