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162 Chapter 7
[Ru2(OOCC(CH3)3)4(H2O)Cl](CH3OH) (SBU-b)
The synthesis was carried out according to the literature. [201] SBU-a (0.3 g, 0.63 mmol)
was dissolved in 60 ml solution of the H2O : CH3OH (1 : 1) mixture. Later, pivalic acid (0.39
g, 3.79 mmol) was added and the resulting mixture was refluxed. The reaction was
finished after 5 hours, when the solution turned to a red-brown color. This solution was
cooled down and left to stay overnight. As a result, red-brown crystals precipitated. The
final product was collected and washed twice with hexane (Yield: 0.37 g).
Figure 7.5. Schematic description of the molecular structure of SBU-b in the solid state obtained
by single crystal structure analysis. Note the half occupied Cl and half occupied O positions at the
apical position of Ru coordination sphere. The oxygen atoms of the methanol molecule in the
asymmetric unit (solvate) were split into two parts due to disorder. Circle with cross: Ru; circle
shaded: Cl; circle shaded bottom right to top left: O; circle with blank: C. Single crystals of SBU-b
were measured at low temperature (101K) while in the literature reference at 295K. The carbon
atoms in CMe 3 were refined isotropically as well as the centrosymmetric structural model with
partial occupation of Cl and O water as in the reference. [201] However, the measurement in the lower
temperature reported here tends to be of better quality.