Chapter 4 - Jacobs University

Chapter 5
Organoruthenium POM
5.3 X-ray crystallography
Crystal data for K 12 Li 15 [{K(H 2 O)} 3 {Ru(p-cymene)(H 2 O)} 4 P 8 W 49 O 186 (H 2 O) 2 ]·87H 2 O (3a): A
brown crystal of 3a with dimensions 0.15 x 0.08 x 0.04 mm3 was mounted in oil on a Hampton
cryoloop for indexing and intensity data collection at 173 K on a Bruker D8 APEX II CCD
single-crystal diffractometer using Mo K a radiation (l = 0.71073 Å). Of the 213856 reflections
collected (2q max = 52.92°, 98.8% complete), 31644 were unique (R int = 0.1473) and 19575
reflections were considered observed (I > 2s(I)). The data were processed using SAINT (from
Bruker AXS) and an absorption correction was performed using the SADABS program
(Sheldrick, G. M.; Acta Crystallogr. 2007, A64, 112). Direct methods were used to locate the
tungsten atoms (SHELXS-97), and the remaining atoms were found from successive Fourier
maps (SHELXL-97). No H or Li atoms were located. In the final refinement, the W, P and Ru
atoms were refined anisotropically; all other atoms were refined isotropically, converging to R =
0.065 (I > 2s(I)) and R w = 0.212 (all data). The two highest peaks in the final Fourier map were
5.86 and 4.2 e - /Å 3 , at 0.74 and 0.35 Å from W25, respectively. The deepest hole was -2.6 e - /Å 3 ,
0.56 Å from K3. The crystallographic data are provided in Table 5.1.
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