240c elemental analyser

Chemicals such as nickel(ii) nitrate hexahydrate, 2-hydroxy-3-methoxybenzaldehyde, 5-nitrosalicylaldehyde, 5-bromo-3-methoxysalicylaldehyde, 2-hydroxy-1-naphthaldehyde, 4-(diethylamino)salicylaldehyde and N,N-dimethyldipropylenetriamine were commercially available reagent or analytical grade chemicals and used as received. 2-Hydroxy-3-methoxy-5-methylbenzaldehyde was synthesized following a literature reported method.^27,28 Solvents were of reagent grade and used without further purification.
Elemental analyses for carbon, hydrogen and nitrogen were carried out in a PerkinElmer 240C elemental analyser. FTIR spectra of the complexes in the range 4000 to 400 cm⁻¹ were measured in a Thermo Scientific Nicolet iS5 FTIR spectrometer using a universal ATR sampling accessory. Direct current (dc) magnetic susceptibility measurements were performed on a Quantum Design MPMS-XL-5 magnetometer under a static magnetic field of 10 kOe in the temperature range of 2 to 300 K. The field dependent magnetization data were collected in the range of dc magnetic field 0–50 kOe at 5 K. All magnetic data were corrected for the sample holder and for the diamagnetic contribution of the samples.

Elemental analysis (C, H and N) was performed using a Perkin-Elmer 240C elemental analyser. IR spectrum in KBr (4500–500 cm⁻¹) was recorded with a Perkin-Elmer Spectrum Two spectrophotometer. Electronic spectra in DMF were recorded on a Shimadzu UV-1700 spectrophotometer. Variable temperature magnetic susceptibility measurements were performed on polycrystalline samples of both complexes (with masses of 37.447 and 36.265 mg, for 1 and 2, respectively) with a Quantum Design MPMS-XL-5 SQUID susceptometer in the temperature range 2–400 K with an applied magnetic field of 0.1 T. The data were corrected for the sample holder and for the diamagnetic contribution of the salts using Pascal's constants (χ_dia = −197.3 × 10⁻⁶ and −204.7 × 10⁻⁶ cm³ mol⁻¹ for 1 and 2, respectively).^{22 (link)}

(NH₄)₆[TeMo₆O₂₄]·7H₂O and Na₃[CrMo₆(OH₆)O₁₈]·8H₂O were prepared according to a reference and confirmed by the IR spectrum.^{24 (link)} Other chemicals were of reagent grade and were used without further purification. FT-IR data were taken on a 60 Scimitar 2000 Near FT-IR Spectrometer by using KBr pellets in the range of 4000–500 cm⁻¹. Thermogravimetric analyses (TGA) were carried out on a Pyris Diamond TG instrument under a flowing N₂ atmosphere with a heating rate of 10 °C min⁻¹. Powder X-ray diffraction data were recorded on an Ultima IV with D/teX Ultra diffractometer at 40 KV and 40 mA with Cu Kα (λ = 1.5406 Å) radiation. C, H, and N elemental analyses were carried out on a Perkin-Elmer 240C elemental analyser. A CHI 760 electrochemical workstation was used for the electrochemical experiments at room temperature.