Micromax 002 ccd diffractometer

The X-ray diffraction experiments were carried out on a Rigaku MicroMax-002+ CCD diffractometer with CuKα radiation (λ=1.54178 Å) at 293 K (Rigaku, Americas, the Woodlands, Texas, USA). Absorption correction and integration of the collected data were handled using the CrystalClear software package (Rigaku Americas). The crystal structures were solved by the direct method followed by Fourier syntheses with SHELXS–97 and then refined by full-matrix least-squares procedures using SHELXL–97 on F² with anisotropic displacement parameters (ADPs) for non-hydrogen atoms. The H atoms were placed in calculated positions and included in the final cycles of refinement in the riding modes²¹ (link). To help data convergence, some restraints were introduced to the refinement of disorders²² . The PLATON program with the probe radius of 1.2 Å was also employed to calculate the volume of the channels where the solvents resided in an asymmetric unit of solvates²³ (link).

Samples were analyzed on a Rigaku MicroMax-002⁺ CCD
diffractometer with Cu–Kα radiation (λ = 1.54178
Å) (Rigaku, Americas, the Woodlands, Texas). Absorption correction
and integration of the collected data were handled using the CrystalClear
software package (Rigaku Americas). The crystal structures were resolved
using the Olex^{2 (link)} crystallography software
platform.^{19 (link)} Structure determination was
achieved by direct method, followed by Fourier synthesis with SIR2008.^{20 (link)} The refinement on F² was performed via the full-matrix least-squares procedures in SHELXL.^{21 (link)} For non-hydrogen atoms, anisotropic displacement
parameters (ADPs) were introduced, whereas hydrogen atoms were refined
isotropically with an isotropic atomic displacement parameter (U_iso) that is 1.2 times the value of the parent
atom. Those from the methyl or hydroxyl groups were assigned 1.5 times
that of the parent atom. The hydrogen atoms were placed in ideal positions
and refined using the riding model, whereas hydrogen atoms involved
in the hydrogen bonding were detected in the experimental electron
density map and refined freely. Refinement of disorders with restraints
was introduced to help data convergence.^{22 (link)}