Advance 3 400 mhz spectrometer

Anhydrous solvents and all reagents were purchased from Sigma-Aldrich (Milan, Italy). All reactions involving air- or moisture-sensitive compounds were performed under a nitrogen atmosphere using dried glassware and syringes techniques to transfer solutions. Nuclear magnetic resonance (¹H-NMR, ¹³C-NMR) spectra were recorded using a Bruker Advance III 400 MHz spectrometer in DMSO-d₆. Chemical shifts are reported in parts per million (ppm) and the coupling constants (J) are expressed in Hertz (Hz). Splitting patterns are designated as follows: s, singlet; d, doublet; t, triplet; q, quadruplet; dd, double of doublet. The assignment of exchangeable protons (OH and NH) was confirmed by the addition of D₂O.

The synthesis of NIK-67 was previously reported by us. Anhydrous solvents and all reagents for the synthesis of AB-118 were purchased from Sigma Aldrich (Milan, Italy). Nuclear magnetic resonance (¹H-NMR, ¹³C-NMR) spectra were recorded using a Bruker Advance III 400 MHz spectrometer in DMSO-d₆. Analytical thin-layer chromatography (TLC) was carried out on Sigma Aldrich silica gel F-254 plates. The melting point (mp) was measured in open capillary tubes with a Gallenkamp MPD350.BM3.5 apparatus and is uncorrected.

The prepared CdS nanoparticles and PHV polymers were analyzed using XRD and NMR, respectively. The CdS was analyzed using a Bruker, Billerica, MA, USA, D8 ADVANCE XRD operating at 35 kV and 40 mA. The XRD spectra were recorded in a 2θ range of 5–80° with a scanning rate of 20°/min. The 1H NMR spectra were recorded using a Bruker Advance III 400 MHz spectrometer at room temperature, and the chemical shifts were referenced to the residual proton resonances.

¹H NMR spectra were collected by using a Bruker Advance III 400 MHz spectrometer (Bruker, Geman) at 298 K; TMS was used as the internal reference. The infrared spectra were recorded by using a Bruker Vertex70 spectrometer (Bruker, Geman) working in attenuated total reflectance mode, the scan range was 4000–400 cm⁻¹. The polymer number-average molecular weight and distribution (also polydispersity index, PDI) was identified by gel permeation chromatography (GPC) with DMF as an eluent (Waters, Massachusetts, Milford, US). UV-vis spectra were measured by using a Persee TU1901 (Persee, Beijing, China) ultraviolet spectrophotometer. Fluorescence spectra were recorded by using a Hitachi F-7000 (Hitachi, Tokyo, Japan) fluorescence spectrometer. Isothermal titration calorimetry (ITC) experiments were performed at 298 K by using a Microcal VP-ITC (Malvern Instruments GmbH, Malvern, England) apparatus at 298 K. Dynamic light scattering (DLS) experiments were performed on a Malvern Zetasizer Nano ZS (Malvern Instruments GmbH, Malvern, England). Samples were filtered through a MILLEX-GV 0.45 µm filter before loading. Transmission electron microscopy (TEM) experiments were performed on a Hitachi-7700-MS electron microscope (Hitachi, Tokyo, Japan). The quantitative evaluation of the cell uptake and release were performed on a BD FACSAria III flow cytometer (BD, San Jose, CA, US).

Samples were exchanged twice with D₂O and were transferred to a 5 mm NMR tube. ¹H NMR spectra were recorded at 323 K using an Advance III 400 MHz spectrometer (Bruker). Chemical shifts are expressed in ppm in reference to water. The HOD signal was not suppressed.

A Bruker Advance III 400 MHz spectrometer was used to record the NMR spectra. The ¹H chemical shifts of molecules are reported relative to the residual solvent protons. A Bruker FTMS 4.7-T Apex II spectrometer was used to perform the mass analysis in the positive mode. UV-vis spectra were measured on a Thermo Fisher Scientific Jasco V730 spectrophotometer. A Bruker TENSOR II spectrometer was used to record the IR spectra, with the following parameters: 16 scans for the background, and 32 scans for a sample, with a resolution of 4 cm⁻¹ in the 4000–600 cm⁻¹ region. Single crystals were measured on a Stoe IPDS2 diffractometer (CuKα1 (λ = 1.5406 Å)) equipped with a cryostat from Oxford Cryosystems. The ShelXT structure solution program was used to solve the crystal structures. We used the Intrinsic Phasing refined with the ShelXL refinement package, using least squares minimization [102 (link),103 (link)]. Data were deposited in the Cambridge Crystallographic Data Centre. The CCDC numbers are 2184717–2184724. The elemental analysis was performed using a LECO CHNS-932 elemental analyzer.

Samples were exchanged twice with D₂O and were transferred into a 5 mm NMR tube. ¹H NMR spectra were recorded at 323 K using an Advance III 400 MHz spectrometer (Bruker). Chemical shifts are expressed in ppm in reference to water. No suppression of the HOD signal was performed.