Oxford diffraction xcalibur ccd diffractometer

Unit cell determination and data collection of the 2–3 compounds were performed at 293 K on an Oxford Diffraction Xcalibur CCD diffractometer (Oxford Diffraction Ltd., Abingdon, UK) with the graphite-monochromated MoKα-radiation (λ = 0.71073 Å). The programs CrysAlis CCD and CrysAlis Red [51 ] were used for data collection, cell refinement, and data reduction. A multi-scan absorption correction has been applied. The structures 2–3 were solved by direct methods using SHELXS-97 and refined by the full-matrix least-squares on F² using SHELXL-97 [52 (link)] and OLEX2-1.5 (OlexSys Ltd., Durham, England) software [53 (link)]. All non-hydrogen atoms in 2 have been refined anisotropically, hydrogen atoms in metal-organic moieties were placed in a calculated position and refined in rigid mode. The structures were verified using the ADDSYM algorithm from the program PLATON [54 (link)] and no higher symmetries were found. Crystallographic and experimental details for 2 and 3 complexes are summarized in Table 1.
CCDC 2099146 [for 2] and 2099147 [for 3] contain the supplementary crystallographic data for this paper. These data can be obtained free of charge from the Cambridge Crystallographic Data Centre.

The X-ray diffraction data were collected at 100(2) K using an Oxford Diffraction Xcalibur CCD diffractometer (Oxford Diffraction Ltd., Abingdon, UK) equipped with a molybdenum sealed X-ray tube (λ = 0.7071 Å), a graphite monochromator, and an Oxford Cryosystems nitrogen gas flow device (Cobra Plus). The CrysAlis [45 ] suite of programs was used for data collection, cell refinement, and data reduction. The data were corrected for Lorentz and polarization effects. A multi-scan absorption correction was applied. The structures were solved using direct methods (SHELXS-97 program) and refined by the full-matrix least squares on F² with the SHELXL-97 program [46 (link)]. All non-H atoms were refined with anisotropic displacement parameters. The H atoms attached to carbon centers were positioned geometrically and refined using a riding model with U_iso(H) = 1.2U_eq(C). The water H atoms were found in the difference-Fourier map and refined with isotropic displacement parameters. Crystal data and structure refinement details for 1 and 2 are given in Table 1. The CIF files for 1 and 2 were deposited at the Cambridge Crystallographic Data Centre (CCDC Nos 2073788–2073789).