Unity inova ddr spectrometer

NMR spectra
were recorded on a Varian Unity Inova DDR spectrometer
(599.9 MHz for ¹H) with a 5 mm ¹H{¹³C/³¹P–¹⁵N} pulse field gradient triple
resonance probe head at 298.15 ± 0.1 K. The solvent was H₂O/D₂O 95:5 (V/V), and the ionic strength was adjusted
to 0.15 mol/L with KCl. The pH values were adjusted with HCl or NaOH
and determined in situ by internal indicator molecules (having ca.
1 mmol/L concentration) optimized for ¹H NMR.^{25 (link),26 (link)} The sample volume was 550 μL (containing ca. 5 mmol/L titrand
substance), and every sample contained ca. 1 mmol/L DSS (3-(trimethylsilyl)propane-1-sulfonate)
as chemical shift reference. The H₂O ¹H signal
was suppressed with a presaturation sequence; the average acquisition
parameters for ¹H measurements are number of transients
= 16, number of points = 65 536, acquisition time = 3.33 s, and
relaxation delay = 1.5 s.

NMR spectra were recorded on a Varian Unity Inova DDR spectrometer (599.9 MHz for ¹H) with a 5 mm ¹H{¹³C/³¹P-¹⁵N} pulse field gradient triple resonance probehead at 298.15 ± 0.1 K. The solvent was H₂O:D₂O 95:5 (V/V), ionic strength was adjusted to 0.15 mol/L with KCl. The pH values were adjusted with HCl or NaOH and determined in situ by internal indicator molecules (at ca. 1 mmol/L) optimized for ¹H NMR [11 , 12 (link)]. The sample volume was 550 μL and every sample contained ca. 1 mmol/L DSS (3-(trimethylsilyl) propane-1-sulfonate) as chemical shift reference. The H₂O ¹H signal was suppressed with a presaturation sequence; the average acquisition parameters for ¹H measurements are: number of transients = 16, number of points = 65536, acquisition time = 3.33 s, relaxation delay = 1.5 s. ¹H-¹³C HSQC measurements were performed with solvent signal presaturation and the following parameters: number of transients = 64, number of increments = 96, number of points = 2884, acquisition time = 149.968 ms, relaxation delay = 1 s.