Luminescence on–off switching via reversible interconversion between inter- and intramolecular aurophilic interactions (original) (raw)
2011, Chemical Communications
S1. Experimental details of 1a and 1b S2. TGA/DSC overlay of 1a and 1b S3. FT-IR spectra of 1a and 1b in KBr S4. 1 H NMR spectrum of 1a and 1b in CDCl 3 /CD 3 OD S5. 13 C NMR spectrum of 1a and 1b in CDCl 3 /CD 3 OD S6. 31 P NMR spectrum of 1a and 1b in CDCl 3 /CD 3 OD S7. 19 F NMR spectrum of 1a in CDCl 3 /CD 3 OD S8. Emission spectra of 1a and 1b in solid state at RT S9. Emission spectra of 1a and 1b in solid state at 77 K S10. Time-dependent emission spectra of 1a in CF 3 CO 2 H and NEt 3 chamber at RT S11. Time-dependent emission spectra of 1a in HCl and NEt 3 chamber at RT Electronic Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2011 S1. Experimental details of 1a and 1b Materials and Instrumentation: Au 2 (dppp)Cl 2 were prepared according to the literature procedure. 2-benzimidazolethiol (BIT) was purchased from Aldrich and was used without further purification. Elemental analyses were performed on crystalline samples by using a Vario-EL analyzer at Center for University-Wide Research Facilities, CBNU. Infrared spectra were obtained with a Thermo Nicolet AVATAR 330 FT-IR spectrophotometer as KBr pellets. 1 H NMR (400 MHz) and 13 C NMR (100 MHz) spectra were recorded with a JEOL JNM AL-400 instrument relative to SiMe 4. 19 F NMR (376 MHz) and 31 P NMR (162 MHz) spectra were reported relative to external CF 3 CO 2 H (100%) and H 3 PO 4 (85%), respectively, with a JEOL JNM AL-400 spectrometer. Emission spectra were obtained using a JASCO FP-6500 spectrofluorometer corrected for instrument response with monochromators positioned with a 2 nm band-pass. Solid-state emission samples were prepared as a 10% (w/w) mixture of the complex in a matrix of finely ground KBr. The melting points were determined with a SRS EZ-Melt MPA-120 melting point apparatus and were uncorrected. Thermal analyses were carried out under a dinitrogen atmosphere at a scan rate of 10 °C/min using a TA Instruments SDT Q20 and DSC Q20. Au 2 (dppp)(BIT) 2 •2CF 3 CO 2 H (1a): To a solution of Au 2 (dppp)Cl 2 (310 mg, 0.35 mmol) in CH 2 Cl 2 (15 mL) was added AgCF 3 CO 2 (156 mg, 0.71 mmol), and the reaction mixture was stirred at RT for 30 min. The suspension was filtered through a pad of celite to remove the AgCl precipitate, and into a suspension of 2-benzimidazolethiol (BIT) (106 mg, 0.71 mmol) in CH 2 Cl 2 (15 mL). The reaction mixture was stirred 2 h at RT. The resulting solution was concentrated to 5 mL, and the addition of Et 2 O (75 mL) gave an off-white precipitate. The precipitate was collected by filtration and washed with Et 2 O. Recrystallization by slow diffusion of Et 2 O into a CH 2 Cl 2 solution gave a white colored product. Yield 76%. Mp 197.6 °C. Anal. Calcd for C 41 H 36 N 4 P 2 S 2 Au 2 •2CF 3 CO 2 H:
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