Crystal handling at low temperatures

Abstract

introductionThe cooling of a crystal in combination with the use of a protecting oil facilitates the handling and transfer to a diffractometer of even very sensitive material. The method is explained and the required device is described in this work. Basic advantages of the technique are simplicity and freedom of access to the sample without the need for sophisticated glassware. Therefore, this technique, suitable for crystal manipulation in the temperature range between room temperature and 193 K, is much more efficient than those involving the use of capillaries.

Low-cost conversion of a coaxial nozzle arrangement into a stationary low-temperature attachment

“…When co is close to zero, single 360 ° rotations in Z can be executed, which is essential for accurate centering of the crystal height. Furthermore, the larger freedom in the goniometer region facilitates structure analyses of temperature-sensitive compounds (Kottke & Stalke, 1993). Implementation of a dualstream rather than a single-stream nozzle allows the distance between the crystal and the nozzle outlet to be moderately varied without this affecting the temperature at the crystal position.…”

Three-Dimensional Lanthanide−Organic Frameworks Based on Di-, Tetra-, and Hexameric Clusters

“…Single-crystals of (CH 3 ) 2 NH 2 [Ln-(pydc) (3) (where pydc 2-) 2,5-pyridinedicarboxylate) were manually harvested from the crystallization vials and mounted on Hampton Research CryoLoops using FOMBLIN Y perfluoropolyether vacuum oil (LVAC 25/6) purchased from Aldrich 18 with the help of a Stemi 2000 stereomicroscope equipped with Carl Zeiss lenses. Data were collected on a Bruker X8 Kappa APEX II charge-coupled device (CCD) area-detector diffractometer (Mo KR graphite-monochromated radiation, λ ) 0.71073 Å) controlled by the APEX-2 software package, 19 and equipped with an Oxford Cryosystems Series 700 cryostream monitored remotely using the software interface Cryopad.…”

mer-Trichloro[2-(phenylamino)pyridinato]oxotungsten(VI)

“…c6 Large black crystalline blocks with an average size of over N7 l mm in each dimension were obtained at room temperature c8 in l0 h. A portion of the crystals was transferred to perfluoro c9 CI0 ether and the specimen was cut from a larger crystal. The Cll crystal used for the X-ray measurements was mounted on a c12 glass fiber using the oil-drop method (Kottke & Stalke, 1993). c13 All reaction steps were carried out under an argon atmosphere using standard Schlenk techniques.…”