Uatr two instrument

A PerkinElmer UATR Two instrument (Perkin Elmer, 8603 Schwerzenbach, Switzerland) was used to record FT-infrared (IR) spectra. Cobalt(II) thiocyanate was bought from Alfa Aesar and used as received. Compounds 1–5 were prepared and characterized as previously described [12 (link)].
All crystal growth experiments were carried out under ambient conditions using identical crystallization tubes (i.d. = 13.6 mm, 24 mL).
Thermogravimetric analysis (TGA) was carried out under nitrogen using a TGA5500 instrument (TA Instruments, New Castle, DE 19720, USA) coupled to a Discovery II MS, Cirrus 3, Mass Spectrometer, DMS (TA Instruments, New Castle, DE 19720, USA). A Barchart scanning method in the mass range 10–125 was applied. For each experiment, the temperature of the TGA instrument was initially stabilized at 30 °C, and then the samples were heated to 80 °C and maintained at this temperature for 30 min. The nature of the solvent lost was identified by mass spectrometry. Afterwards the sample was cooled to room temperature (ca. 22 °C) and placed in contact with vapors of CHCl₃, CDCl₃ or CH₂Cl₂ for 24 h. TGA was then repeated using the above procedure.

¹H, ¹³C{¹H} and 2D NMR spectra were recorded at 298 K on a Bruker Avance iii-500 spectrometer (Bruker BioSpin AG, Fällanden, Switzerland) equipped with a BBFO probehead. The ¹H and ¹³C NMR chemical shifts were referenced with respect to residual solvent peaks (δ TMS = 0). A Shimadzu LCMS-2020 instrument (Shimadzu Schweiz GmbH, 4153 Reinach, Switzerland) was used to record electrospray ionization (ESI) mass spectra, and a Bruker maXis 4G QTOF (Bruker BioSpin AG, Fällanden, Switzerland) instrument for HR ESI mass spectra. A PerkinElmer UATR Two instrument (PerkinElmer, 8603 Schwerzenbach, Switzerland) and a Shimadzu UV2600 (Shimadzu Schweiz GmbH, 4153 Reinach, Switzerland) spectrophotometer were used to record FT-IR and absorption spectra, respectively.
Bis(pinacolato)diboron, 4-bromo-2,5-dimethoxybenzaldehyde, 2-acetylpyridine, 3-acetylpyridine, and [Pd(dppf)Cl₂] were purchased from Fluorochem (Chemie Brunschwig AG, 4052 Basel, Switzerland), 4-acetylpyridine and Fe(BF₄)₂·6H₂O from Sigma Aldrich (Sigma Aldrich Chemie GmbH, 89,555 Steinheim, Germany), and Na₂CO₃ and FeCl₂·4H₂O from Acros Organics (Fisher Scientific AG, 4153 Reinach, Switzerland). These chemicals were used as received.

¹H and ¹³C NMR spectra were recorded on a Bruker Avance iii-500 spectrometer (Bruker BioSpin AG, Fällanden, Switzerland) at 298 K. The ¹H and ¹³C NMR chemical shifts were referenced with respect to residual solvent peaks (δ TMS = 0). A Shimadzu LCMS-2020 (Shimadzu Schweiz GmbH, 4153 Reinach, Switzerland) instrument was used to record electrospray ionization (ESI) mass spectra. A PerkinElmer UATR Two instrument (Perkin Elmer, 8603 Schwerzenbach, Switzerland) and Shimadzu UV2600 (Shimadzu Schweiz GmbH, 4153 Reinach, Switzerland) or Cary 5000 (Agilent Technologies AG, 4052 Basel, Switzerland) spectrophotometers were used to record FT-infrared (IR) and solution absorption spectra, respectively.
3-Acetylpyridine, 4-n-octyloxybenzaldehyde and 4-n-nonyloxybenzaldehyde were purchased from Acros Organics (Chemie Brunschwig AG, Basel, Switzerland) and were used as received. Ligands 6 [25 (link)] and 7 [11 (link)] were prepared as previously reported.