Ipds 2t diffractometer

Crystals of 6 and 7 were grown by slow evaporation of a mixed acetonitrile/ethanol solvent system and subjected to diffraction experiments on a STOE-IPDS-2T-diffractometer. Graphite-monochromated Mo Kα radiation (λ = 0.71073 Å) was used throughout. The data were processed with X-AREA and corrected for absorption using STOE X-Red32 [67 ]. The structures were solved by direct methods (SHELXS-2013) [68 (link)] and refined by full-matrix least-squares on F². However, the quality of the refinement for the two compounds was very low. The ClO₄⁻ anions and solvate molecules could not be located, and so the structures can only serve to validate the atom connectivity of the complex cations.

Single-crystal X-ray diffraction measurements were performed on a STOE IPDS-2T diffractometer with graphite monochromated Mo-Kα radiation. Single crystals were chosen using a polarizing microscope and were mounted on glass fibers for data collection. Cell constants and orientation matrices were obtained by least-squares refinement against setting angles for all reflections. Diffraction data were collected as a series of 1° ω scans and integrated using the Stoe X-AREA software package.³¹ Lorentz and polarization corrections were applied to the data and a numerical absorption correction was applied using X-RED³² and X-SHAPE.³³ The structures were solved by direct methods³⁴ and subsequent difference Fourier maps and then refined on F² by full-matrix least-squares with anisotropic displacement parameters for all non-H atoms.³⁵ The atomic scattering factors were taken from International Tables for X-ray Crystallography.³⁶ All refinements were performed within the Stoe X-STEP32 structure evaluation package.³⁷