ABSTRACT
In situ single-crystal diffraction experiments provide researchers with the opportunity to study the response of crystalline systems, including metal–organic frameworks and other nanoporous materials, to changing local microenvironments. This paper reports a new environmental control cell that is remarkably easy to use, completely reusable, and capable of delivering static or dynamic vacuum, liquids or gases to a single-crystal sample. Furthermore the device is nearly identical in size to standard single-crystal mounts so a full unrestricted range of motion is expected for most commercial goniometers. In situ single-crystal X-ray diffraction experiments performed under dynamic gas-flow conditions revealed the cell was capable of stabilizing a novel metastable intermediate in the dehydration reaction of a previously reported metal–organic framework.
Image of the assembled ECC mounted on a standard goniometer head. Right: exploded view of ECC components: a, bent 18 g needle; b, ECC body; c, capillary retaining screw; d, o-ring; e, capillary (shortened and sealed with glue); f, set screw; g, sample mounted on thin glass fibre.
Cut-away model of the ECC base with dimensions in millimetres. Colours have been added to the wireframe for clarity. The blue wireframe region is threaded with 5/16–24 threads. The grey circle indicates the approximate location of the needle within the notch. The set screw is located within the 1.66 mm lip.
Jordan M. Cox,a Ian M. Walton,a Cassidy A. Benson,a Yu-Sheng Chenb and Jason B. Benedicta*
aDepartment of Chemistry, University at Buffalo, SUNY, Natural Sciences Complex, Buffalo, NY 14260-3000, USA, and bChemMatCARS, Center for Advanced Radiation Sources, 9700 South Cass Avenue, Building 434D, Argonne, IL 60532, USA
*Correspondence e-mail: jbb6@buffalo.edu
DOI: 10.1107/S160057671500432X
J. Appl. Cryst. (2015). 48, 578–581