Raxis spider ip diffractometer

A suitable crystal of the compound Mo₆-Q-NO₂ was covered with petroleum jelly, mounted onto glass fibers, and transferred directly to a Rigaku RAXIS-SPIDER IP diffractometer. Data collection, data reduction, cell refinement, and experimental absorption correction were performed with the software package of Rigaku RAPID AUTO (Rigaku, 1998, Ver2.30). Structures were solved by direct methods and refined against F² by full matrix least squares. All non-hydrogen atoms, except disordered atoms, were refined anisotropically. Hydrogen atoms were generated geometrically. All calculations were performed using the SHELXTL V. 5.10 program43 .

The single crystal of NSeD was obtained in the process of vacuum sublimation. Low temperature (104.6 K) single-crystal X-ray experiments were performed on a Rigaku RAXIS-SPIDER IP diffractometer with graphite-monochromatized Mo_Kα radiation (λ = 0.71073 Å). Data collection and reduction, cell refinement, and the experiential absorption correction for all compounds were performed with the Rigaku RAPID AUTO software package (Rigaku, 1998, Version 2.30). The structure was solved using direct methods and refined against F2 using full-matrix least-squares techniques. CCDC ; 1402824 contains the supplementary crystallographic data for this paper.†

Single crystals of Ir1 that were suitable for an X-ray crystallographic study were grown from dichloromethane-toluene (1:1, v/v) at room temperature. An orange crystal was recorded on a Rigaku R-AXIS SPIDER IP diffractometer (MoKα, λ = 0.71073 Å) at 150(2) K. An absorption correction was applied using SADABS program59 (link). The structure solution and full-matrix least-squares refinement based on F2 for Ir1 were performed with the SHELXS-2014 and SHELXL-2014 program60 (link), respectively, incorporated into the OLEX2 program package. Anisotropic thermal parameters were applied to all of the non-hydrogen atoms. All of the hydrogen atoms were included in calculated positions and were refined with isotropic thermal parameters riding on those of the parent atoms. Detailed crystallographic data for the crystal structural analysis were deposited with the Cambridge Crystallographic Data Centre, CCDC 1046980 (Ir1), containing the supplementary crystallographic data for the present study. The data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.