Flash 2000 analyser

A Waters ESI⁺ TOF Micro-mass LCT Premier Spectrometer operated in the positive ion mode was used to record low-resolution ESI⁺ mass spectra of the ligands and complexes. Mass spectra for synthesised complexes namely, bpqPtCl₂, dmbpqPtCl₂ and bbqPtCl₂ are presented in ESI Fig. S13, S14 and S15,† respectively. Elementary compositions of the ligands and complexes were determined on a Thermo Scientific Flash 2000 analyser. ¹⁹⁵Pt-NMR data were obtained from a Bruker Avance DPX 400 spectrometer at a frequency of 400 MHz using either 5 mm BBOZ probe or a 5 mm TBIZ probe at 30 °C. Kinetic and pK_a measurements were recorded on a Varian Cary 100 Bio UV-Visible spectrophotometer coupled to a Varian Peltier temperature controller having an accuracy of ±0.05 °C. A Shimadzu UV-1800 UV-visible spectrophotometer fitted with CPS 240A was used for study the binding interactions of the Pt(ii) complexes with CT-DNA and BSA. The temperature of the instrument was controlled to within ±0.1 °C by the Peltier effect. Emission spectra were recorded using a PerkinElmer LS 45 Fluorescence Spectrometer. The pH of the solutions was recorded on a Jenway 4330 conductivity & pH meter equipped with 4.5 μm glass electrode. The pH meter was calibrated at 25 °C using standard buffer solutions at pH values of 4.0, 7.0 and 10.0.

Commercially available solvents and chemicals were obtained from suppliers and used to execute this work as received unless otherwise mentioned. All the reactions were performed on a Monowave 300 microwave synthesizer (Anton Paar) by employing a glass vial G10. TLC analysis was performed using silica gel GF-254 from SRL. Stuart digital melting point apparatus (SMP10) was used for the measurement of melting points, which are uncorrected. FTIR spectra were recorded in potassium bromide pellets on a Perkin-Elmer 10.4.00 IR spectrophotometer. ¹H-NMR and ¹³C-NMR spectral analysis were carried out on Bruker (Avance-II 400 MHz, Varian-AS400 NMR) spectrometers using TMS as an internal standard and DMSO-d₆ as a solvent. Crystal data were collected with a SuperNova diffractometer, single source at offset/far, with a HyPix3000 detector (CCD) at 293 K using graphite monochromated MoKα radiation (λ = 0.71073 Å). Elemental analysis was performed on a Perkin-Elmer-2400 CHN/S analyser and Thermo Scientific (FLASH 2000) analyser while high resolution mass spectra were recorded on an ORBITRAP mass analyser (Thermo Scientific, Q Exactive) under electrospray ionisation (ESI) conditions.