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In the present structural determination, many atoms could not be refined anisotropically. There were some very large, anisotropic displacement parameters (for example, Mo16 and O16, Such very large anisotropic displacement parameters and not-well-lowered R indexes (R1, 0.11 and wR2, 0.29) often are evidence of disorder and/or twinning. We tested some twinning (merohedral and pseudomerohedral twinning such as a (100) twin in P21/n) and further disorder (for example, ones concerning Mo16 and O16, see Figure S1, Supporting Information for atom-labeling) models, but no improvements were obtained in the structure refinements. In the final difference map, the deepest hole was -3.44 e Å-3 near the Mo16 position and the highest peak 5.19 e Å-3 near the P3 position. The highest peak was tested as the P atom, which gave an atomic occupancy of almost zero. It must be added that meas
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-3 near the P3 position. The highest peak was tested as the P atom, which gave an atomic occupancy of almost zero. It must be added that measurements with the use of Cu Kα radiation (1.5418 Å) gave no improvements in the structure refinements.
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17
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57949098734
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The present structural solution showed that there still was 4400 Å3 of void in the unit cell, indicating the presence of a lot of diffuse solvent (acetonitrile molecules, We estimated the existence of ca. 40-50 acetonitrile molecules in the solvent-accessible void, since one acetonitrile molecule was calculated to occupy ca. 100 Å3. These acetonitrile molecules were easily released from the crystal, because the elemental analysis data were in good agreement with those for (Pr 4N)8[(HPO3)2(P2O 7) Mo30O90, without acetonitrile
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90] (without acetonitrile).
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