Advance 300 mhz

Solvents and reagents used for the synthetic work were purchased from Aldrich, TCI, Acros Organics or Alfa Aesar and used without further purification. Compounds 3–5 were prepared as reported previously [58 (link),59 (link),60 (link),61 (link)]. NMR spectra were recorded on a Bruker Advance-300 MHz instrument. The NMR spectra were referenced to residual solvent peaks and the spectroscopic solvents were purchased from either Cambridge Isotope Laboratories or Deutero GmbH Laboratories. The Q-TOF HRMS data was recorded on a Waters (Xevo G2-XS Tof) instrument. UV/Vis spectra were measured on a Mega-800 (SCINCO) spectrometer. Fluorescence spectra were measured on a RF-6000 (SHIMADZU) spectrometer. TLC analyses were carried out using Sorbent Technologies silica gel (200 mm) sheets. Column chromatography was performed on Sorbent silica gel 60 (40–63 mm). For computations, PCModel was used to locate the lowest energy conformation for the free ligand and various ligand anion complexes [62 ]. This was done by sampling structures taken from 50 ps molecular dynamics runs using the Merck Force Field 94 model in vacuo [63 (link)]. The energies for the lowest energy forms of each species were used to compute interaction energies:

The solid copolymer samples were tested using a Galaxy series FT-IR 5000 spectrophotometer at 2 cm⁻¹ resolution in the wavenumber range 400–4000 cm⁻¹. ¹H-NMR spectra were recorded on a Bruker Advance 300 MHz instrument by using D₂O as a solvent. Copolymer thermal stability was assessed using thermogravimetric analysis (TGA) using a Mettler TGA Q5000 TA under nitrogen gas in the temperature range 50–800 °C with a heating rate of 10 °C/min. The weight-average molecular weight (Mw), number-average molecular weight (Mn), and polydispersity index (PDI) of the copolymers were determined using gel permeation chromatography by a K-2301 (KNAUER) detector. The glass transition temperature Tg was recorded on Mettler DSC 2500 TA differential scanning calorimeter at a scanning rate of 10 °C/min under a nitrogen atmosphere. The X-ray diffraction (XRD) of nanocomposites was collected in data using a XPERT-PRO X-Ray diffractometer using Cu Kα radiation (40 kV, 30 mA). The samples were scanned in the range from 2θ = 5° to 15° using step scan of 0.05° for a time interval of 10 s. Also scanning electron microscope (TESCAN, Mira 3-XMU) was used for assigning the surface morphology of the prepared nanocomposites. The contact angle was measured using a digital camera equipped on contact angle tester (JIKAN, CAG-20 SE).

PHBV samples were dissolved in CDCl₃, and ¹H- and ¹³C-nuclear magnetic resonance (NMR) spectra were recorded on an Advance Bruker 300 MHz and 500 MHZ spectrometer (Billerica, MA, USA) at room temperature, respectively. Spectra were analyzed using TopSpin V3.6.2 software (Billerica, MA, USA). The ¹H-NMR spectra obtained for the PHBV samples were used to estimate monomer unit content. The molar fraction of the 3HV unit of the fractionated PHBV samples was estimated from the relative integrated CH₃ (V5) resonance. ¹³C-NMR spectra was used to determine the sequence distribution of 3HV and 3HB in PHBV as previously described [8 (link),28 (link),29 (link)].