Pyris 1 thermogravimetric analyser

Reagents and solvents were obtained from Sigma-Aldrich, Alfa Aesar, Acros Organics, Fisher Scientic, Fluorochem or Manchester Organics, and were used without additional purication. Samples used for elemental analysis, thermogravimetric analysis and laboratory powder X-ray diffraction were ground into a powder using a mortar and pestle immediately prior to analysis, to ensure consistency of solvent content in the bulk material. For solution-phase NMR spectroscopic characterisation, the sample (ca. 3 mg) was acid-digested in 50 mL deuterium chloride (35% in D 2 O) in 1 mL DMSO-d 6 . Thermogravimetric analysis was performed in air using a PerkinElmer Pyris1 Thermogravimetric Analyser. Elemental analysis was performed by combustion in pure oxygen using a Perki-nElmer 2400 CHNS/O Series II Analyser or an Elementar Vario MICRO cube analyser. NMR spectroscopy (400 MHz) was performed using Bruker AVANCE III 400 HD or AVANCE 400 HD spectrometers.

Routine 1 H NMR spectra were obtained on a Varian Unity INOVA spectrometer operating at an equivalent 1 H frequency of 500 MHz performed at 30 °C.
The GPC system was composed of a Waters 515 HPLC pump, a Waters 717plus Autosampler, a column system of 2 Waters Styragel HR columns (HR1 and HR4), a Jetstream thermostat and an Agilent Infinity 1260 Differential Refractometer detector. Distilled tetrahydrofuran was used as eluent with a flow rate was 0.3 mL/min.
Thermogravimetric analyses were performed in air (50 ml/min) using a Perkin Elmer Pyris 1 Thermogravimetric Analyser over a temperature interval 30-600 °C at a heating rate of 10 °C min -1 .