Sc-XRD experiments for 1·4H2O and 1 were performed using a Bruker D8 Quest Eco diffractometer (Mo Kα sealed tube radiation source, Triumph® monochromator). Single crystals of 1·4H2O were moved directly from the mother liquor into NVH oil to avoid loss of the crystallization solvent. A single crystal of 1 was prepared in situ by heating 1·4H2O mounted on the goniometer head in a dry nitrogen stream using a Cryostream device (Oxford Cryosystems). Absorption corrections, data reduction and unit cell refinements were performed using SADABS and SAINT programs included in the Apex3 suite. The structures were solved using intrinsic phasing and refined anisotropically using weighted full-matrix least-squares on F2.66–68 (link) Hydrogen atoms of the ligands were placed in calculated positions and refined as riding on the parent atoms. Structural diagrams were prepared using Mercury CSD 2020.3.0.35 (link) CCDC 2240344 (1·4H2O at 200 K) and 2240345–2240347 (1 at 200, 140 and 80 K, respectively) contain the supplementary crystallographic data for this paper.
Cryostream device
Manufactured by Oxford Cryosystems
The Cryostream device is a laboratory equipment designed for low-temperature sample manipulation and analysis. It provides a precisely controlled flow of cryogenic gas to maintain a stable and uniform temperature environment around a sample. The Cryostream is used to facilitate various scientific investigations and experiments that require temperature-sensitive samples or conditions.
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Lab products found in correlation
2 protocols using cryostream device
1
Single Crystal X-Ray Diffraction Analysis
2
Birefringence Characterization of Single Crystals
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Single crystals showing birefringence under polarised light were isolated in Paratone-N oil, then mounted on a suitable crystal mounting loop. Diffraction data at 100K were collected using a Rigaku Synergy diffractometer equipped with a Cu microsource, a HyPix detector and an Oxford Cryosystems Cryostream device. Crystal structures were solved using ShelXT 32 and refined using ShelXL 33 (running as part of the Olex2 34 system) and crosschecked with the Cambridge Structural Database (CSD) database ,35 then rendered using Mercury. 36 The positions of hydrogen atoms were determined directly from the observed electron density. Hydrogen atoms attached to carbons were treated with a riding ('AFIX') model, whilst hydrogen atoms attached to O or N atoms were allowed to refine freely, ensuring that the co-crystal or salt nature of the materials was directly determined. Fourier-Transform Infrared Spectroscopy (FTIR) FTIR spectra were collected using a Perkin-Elmer 100 FTIR Spectrometer equipped with a diamond attenuated total reflectance (ATR) accessory (Shelton, Connecticut, USA). 16 scans were made, with transmission recorded over the range 650-4000 cm À1 with a resolution of 4 cm À1 .
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