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The triclinic structure of NaH 2 [PW 12 O 40 ] ·  x H 2 O ( x  = 12–14) has been determined and the results are compared with those of K eggin  (1933) and N oe -S pirlet  et al . (1974). Crystal data:  P [unk],  a  = 14.06(1) Å,  α  = 93.2(1)°,  b  = 14.07(1) Å,  β  = 112.7(3)°,  c  = 14.03(1) Å,  γ  = 118.1(3)°,  V  = 2163 Å 3 ,  Z  = 2,  D  x  = 4.78 g · cm −3  (for  x  = 12). 5375 independent reflections were measured by a Philips PW 1100 four-circle diffractometer (Mo Kα  radiation, graphite monochromator,  ω -2 θ  scan). The W positions were taken from a Patterson map, the other ones from a  Δ -Fourier map. The O and Na positions came out clearly, but the H 2 O molecules seem to be bound zeolithelike and the correct number of H 2 O molecules remains uncertain. Final  R  = 12.9% (without absorption correction). The pseudosymmetry [unk]3 m  of the complex is quite well obeyed. As compared with the data of K eggin  (1933), the O atoms are shifted considerably, but the arrangement of the W atoms is the same within the limits of error. Average distances P–O = 1.545 Å, O–W: 2.42 Å (3W + 1P), 1.91 Å (2W) and 1.69 Å (1W).

Die Struktur des Kegginkomplexes [PW 12 O 40 ] 3− am Beispiel des triklinen NaH 2 [PW 12 O 40 ] · x H 2 O ( x = 12–14)