Vertex 80 spectrometer

Step-scan UV–vis spectroscopy: Step-scan UV–vis spectroscopy was performed using a Vertex 80 spectrometer (Bruker) with a Si diode detector. For samples containing pristine BINAP on quartz substrates was prepared using a chemical vapour deposition (CVD) technique. In this study, a third harmonic of a Nd:YAG laser (Continuum, Surelite) at 355 nm was used as the pump pulse, which has a duration of 15 ns and a repetition rate of 10 Hz. The background reduction and optimization of pumping power required various combinations of interference filters and were necessary to avoid thermal noise and sample decomposition. A typical excitation energy was adjusted to lower than 200 mJ·cm⁻². An optimized laser pulse had a decent signal-to-noise ratio to avoid damaging the sample. Moreover, the excitation source was synchronized with the spectrometer and was set at an accurate 45° with respect to the UV–vis probe beam to maximize the pump–probe overlap. In addition, the visible source (tungsten lamp, 24 V, 150 W) was employed as an externally source coupled with a water cooling unit and power supply. During the measurement, the entire UV–vis compartment was purged with 2 bar nitrogen at room temperature.

For FTIR spectroscopy, isolated fibrils or monomers were spotted onto a thin KBr pellet and were subjected to dry under an IR lamp. Then the spectrum was collected using a Bruker VERTEX 80 spectrometer attached with a DTGS detector at the frequency range of 1800–1500 cm^–1, corresponding to amide I stretching frequency, with a resolution limit of 4 cm^–1. The recorded spectrum was deconvoluted at the frequency range 1700–1600 cm^–1, using Fourier Self Deconvolution (FSD) method and the deconvoluted spectrum was fitted using the Lorentzian curve fitting method using OPUS-65 software (Bruker, Germany) according to the manufacturer’s instructions. Independent sets were performed thrice for each sample.

The in situ static transmission IR experiments were conducted in a home-built cell housed in the sample compartment of a Bruker Vertex 80 spectrometer, equipped with an MCT detector and operated at 4 cm⁻¹ resolution. The powder sample was pressed onto a tungsten mesh which, in turn, was mounted onto a copper heating assembly attached to ceramic feedthrough. The sample could be resistively heated or cooled with liquid nitrogen, and the sample temperature was monitored by a thermocouple spot welded onto the top center of the W grid. The cold finger on the glass bulb containing CO was cooled with liquid nitrogen to eliminate any contamination originating from metal carbonyls, while NO was cleaned with multiple freeze–pump–thaw cycles. Prior to spectrum collection, a background with the activated (annealed, reduced, or oxidized) sample in the IR beam was collected. Each spectrum reported is obtained by averaging 64 scans.
HAADF-STEM was performed with an FEI Titan 80–300 microscope operated at 300 kV. The instrument is equipped with a CEOS GmbH double-hexapole aberration corrector for the probe-forming lens, which allows for imaging with 0.1 nm resolution in scanning transmission electron microscopy mode (STEM). The images were acquired with a high angle annular dark-field (HAADF) detector with an inner collection angle set to 52 mrad.

We employed synchrotron-radiation-sourced FT-IR spectroscopy (SR-μFTIR)
to characterize the biochemical compositions of the untreated and
treated worms. Worms at the fully grown adult stage are more difficult
to penetrate by the incident rays. Therefore, to have a better intensity
of the FTIR spectra, ∼500 L3 stage worms are treated with the
substances in Milli-Q water for 16 h, washed by centrifugation, transferred
dropwise onto a 9 mm CaF₂ window (∼45 worms per
window), and vacuum-dried. The SR-μFTIR analysis was conducted
at the MIRAS beamline at ALBA synchrotron, Spain using a Hyperion
3000 Microscope coupled to a Vertex 80 spectrometer (Bruker) equipped
with 36× magnification objective from 900–4000 cm^–1. The spectra were collected in transmission mode
using an MCT detector at 4 cm^–1 spectral resolution
and 8 × 8 μm² aperture dimensions. Background
signal was scanned in each CaF₂ window from an area free
of worms. FTIR spectra were extracted using OPUS 7.5 (Bruker), noise
removal, baseline correction, and application of Savitsky–Golay
second derivative were performed using Unscrambler and Origin 2019b.
Relative absorbance ratios were calculated from the second derivative
obtained from the FTIR spectral data. Four ratios, namely, lipid oxidation
(A1740/A2920), saturation (A2920/A2960), and unsaturation (A3012/A2920)
levels were evaluated.

The attenuated total reflection
infrared spectra (ATR-FTIR) were obtained by using a Bruker Vertex
80 spectrometer (Billerica, MA). A DTGS detector was used to acquire
data at 4 cm^–1 resolution. The scans were 2 min
long for both sample and background and had a 5 kHz sampling rate.
The protein solutions were sampled at a 45° angle of incidence
by using a Pike Technologies VeeMax II ATR accessory with a 45°
ZnSe crystal (Madison, WI). For each of the tested protein solutions,
6 sample and 6 buffer scans were acquired relative to the empty crystal
and averaged to produce the spectra. Buffer subtraction, data manipulation,
and export were carried out with Bruker Opus 7.5 software. Spectral
derivatives were determined using Opus 7.5 after the spectra were
min-max normalized between 1720 and 1600 cm^–1.

All reagents are analytically pure grade in the experiment and are not further purified for use. Thermogravimetric analysis was measured on a NETZSCH STA 449 F5 Jupiter TGA analyzer (Selb, Germany) using an empty Al₂O₃ crucible as the standard. Measuring temperature ranges from 25 to 800 °C with a heating rate of 10 °C min⁻¹ under N₂ atmosphere. Powder X-ray diffraction patterns of the title complex were obtained using a Shimadzu XRD-6000 X-ray diffractometer (Kyoto, Japan) with Cu-Kα (λ = 1.5418 Å) radiation at room temperature and 2θ ranging from 5° to 50°. Perkin Elmer (Waltham, MA, USA) 240C elemental analyzer was used to obtain elemental analyses of complex 1. Infrared spectra were obtained on a Bruker VERTEX 80 spectrometer (Billerica, MA, USA) in the 4000–400 cm⁻¹ region. Fluorescence data were collected on the Perkin Elmer LS55 Fluorescence Spectrophotometer.