Ttk 450

The crystallinity and the possible polymorphic transformation of PMOL were evaluated by using a Bruker D8 Advance (Germany) in theta-theta reflection mode with copper anode. A parallel beam Goebel mirror with 0.2-mm exit slit and LynxEye sensitive detector opening at 3 degrees with 176 active channels was used. Each sample was scanned from 2 to 40 2θ with a step size of 0.02 2θ. An Anton Paar TTK450 non-ambient sample chamber was used to achieve the variable temperature with a heating rate of 0.2°C/s. Data collection and interpretations were performed using DiffracPlus and the the EVA V.16 program, respectively (18 ).

All the reagents and solvents were commercially available and used as supplied without further purification. ICP-AES (IRIS Intrepid II XSP, Thermo Electron Corporation) was used for the analysis of metal ion concentrations. UV-Vis absorption spectra were collected by an Agilent Cary 5000 UV-Vis-NIR Spectrophotometer. TEM, HR-TEM and STEM images were measured using a JEOL JEM-2200FS with image Cs-corrector equipped (National Institute for Nanomaterials Technology (NINT), Korea). SEM images were collected by a JSM 7800F PRIME scanning electron microscope operating at 1 kV. Powder XRD patterns were obtained on a Rigaku Smartlab system equipped with a Cu sealed tube (wave length = 1.54178 Å) and a vacuumed high-temperature stage (Anton Paar TTK-450). The following conditions were used: 40 kV, 30 mA, increment = 0.01°, and scan speed = 0.3 s per step. NMR data were recorded on a Bruker DRX500 spectrometer. Small-angle X-ray scattering (SAXS) measurements were carried out using the 4C SAXS II beamline (BL) of the Pohang Light Source II (PLS II) with 3 GeV power and an X-ray beam wavelength of 0.734 Å at the Pohang University of Science and Technology (POSTECH), Korea. The magnitude of the scattering vector, q = (4π/λ) sin θ, was 0.1 nm^–1 < q < 6.50 nm^–1, where 2θ is the scattering angle and λ is the wavelength of the X-ray beam. All scattering measurements were carried out at 25 °C.

X-ray powder diffraction (XRPD)
analyses were performed on a PANalytical X’Pert Pro automated
diffractometer with an X’Celerator detector in Bragg–Brentano
geometry, using Cu Kα radiation (λ = 1.5418 Å), Soller
slit of 0.04 rad, divergence slit of 1/4°, antiscatter slit of
1/2°, 40 mA, and 40 kV. Variable temperature XRPD were collected
with the same instrument equipped with a non-ambient chamber Anton
Paar TTK 450. TOPAS V7 was used for the Pawley refinement and determination
of the average crystal domain size.^{34 (link),35 (link)}

X-ray powder
diffractograms in the 5–40° 2θ range were collected
on a PANalytical X’Pert PRO automated diffractometer equipped
with an X’Celerator detector and an Anton Paar TTK 450 system
for measurements at controlled temperature. The data were collected
in open air in Bragg–Brentano geometry using CuKα radiation
without a monochromator.