X-ray structure determination of alkali metal-based coordination compounds. The single crystals of 1•5H2O, 2•3H2O and 3•3H2O, were selected under Paratone-N oil, mounted on the nylon loops and positioned in the cold stream on the diffractometer. The SCXRD data were processed with CrysAlisPro, Data Collection and Processing Software for Agilent X-ray Diffractometers. The structures 1 • 5 H2O, 2 • 3 H2O and 3 • 3 H2O were solved by direct methods using the SHELXT program and were refined by full matrix least-squares on F2 using the program SHELXL. implemented in the OLEX2 or WinGX 66 suite. All non-hydrogen atoms were refined with anisotropic displacement parameters. H atoms on C atoms were added to the structure model at geometrically idealized coordinates and refined as riding atoms. H atoms of H2O molecules were located from a Fourier map (Tables ). Crystallographic data (excluding structure factors) for the structure reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as a supplementary publication. Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB21EZ, UK (fax: (+44)1223-336-033; e-mail: deposit@ccdc.cam.ac.uk). CCDC: 2359247 (1 • 5 H2O), 2359249 (2 • 3H2O),