Chapter 4 - Jacobs University
Chapter 4 - Jacobs University
Chapter 4 - Jacobs University
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<strong>Chapter</strong> 2<br />
Experimental<br />
2.0.1 Reagents<br />
<strong>Chapter</strong> 2<br />
Experimental<br />
All chemicals were purchased from well known chemical companies, and used as received:<br />
CuCl 2·2H 2 O, NaN 3 , UO 2 (NO 3 ) 2·7H 2 O, H 2 O 2 (30%) and HfCl 4 (anhydrous) were purchased from<br />
Fluka Chemie, Na 2 WO 4·2H 2 O, YCl 3·6H 2 O, CuBr 2 (anhydrous), MnCl 2 ×4H 2 O and ZrCl 4<br />
(anhydrous) were purchased from Riedel-de haën, FeCl 3 ×6H 2 O, Fe(ClO 4 ) 3 ×xH 2 O, CoCl 2 ×6H 2 O,<br />
NiCl 2 ×6H 2 O and [Ru(p-Cyemen)Cl 2 ] 2 were<br />
purchased from Aldrich Chem.Co, NaVO 3 and<br />
VOSO 4·xH 2 O were from Alfa Aesar. FeSO 4·7H 2 O and D 2 O were purchased from AppliChem.<br />
2.1 Instrumentation<br />
2.1.1 Infrared spectroscopy<br />
Infrared spectra with 4 cm -1<br />
resolution were recorded on a Nicolet Avatar 370 FT-IR<br />
spectrophotometer as KBr pellet samples. The following abbreviation was used to assign the<br />
peak intensities: w = weak; m = medium; s = strong; vs = very strong; b = broad; sh = shoulder.<br />
2.1.2 Single crystal X-ray diffraction<br />
X-ray diffraction data collection was carried out on a Bruker D8 SMART APEX CCD single<br />
crystal diffractometer equipped with a sealed Mo anode tube. The SHELX software package was<br />
used in order to solve and refine the structures. Direct method solutions located the heaviest<br />
atoms and remaining atoms were found in subsequent Fourier difference syntheses. Refinements<br />
were full-matrix least-squares on F 2 for structures having not more than 1200 parameters, and<br />
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