The crystal structure of [(CH3)4N]4Na2H[alpha-PW11O39].8H2O has been determined by using the Weissenberg camera at the BL04B2 beamline of SPring-8, revealing that it contains a disorder-free lacunary [alpha-PW11O39]7- anion with one sodium cation embedded into its lacuna that links the oxometalate building blocks into a one-dimensional chain, which is then woven into a three dimensional latticework by another Na+.
An imaging plate Weissenberg camera was installed in the BL04B2 beamline of SPring-8 aiming at automated crystal structure determinations of small molecules. Since this beamline is designed to provide X-rays with the energies higher than 37 keV (λ < 0.33 Å), this camera is advantageous in crystal structure analyses of heavily X-ray absorbing materials. The title crystal structure analysis led to precise positional parameters and well-behaved displacement parameters not only for heavy atoms but also for light atoms.
As revealed by single crystal XRD, the compound crystallizes in the monoclinic space group Cc at 153 K with Z = 4. The structure contains a disorder-free lacunary [α-PW 11 O 39 ] 7anion with one Na + cation embedded into its lacuna that links the oxometalate building blocks into a one-dimensional chain, which is woven into a three-dimensional network by another Na + . -(HONMA, N.; KUSAKA, K.; OZEKI*, T.; Chem.
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