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The crystal structure of (NH 4 ) 4  · [Mo 8 O 24+ x  (O 2 ) 2− x  (H 2 O) 2 ] · 4H 2 O ( x  = 0.8) has been determined from single-crystal X-ray diffraction data. The yellow compound crystallizes in the monoclinic space group  P 2 1 / n  with  a  = 10.427(3) Å,  b  = 7.914(5) Å,  c  = 18.103(3) Å,  β  = 96.10(2)°,  V  = 1485.5(9) Å 3  and  Z  = 2. Full-matrix least-squares refinement of 213 structural parameters gave  R ( F ) = 0.034 ( R w  ( F ) = 0.042) for 2630 observed [ I  &gt; 3 σ ( I )], independent reflections. The formula implies that part of the diaquatetracosaoxodiperoxooctamolybdate(VI) ions have been replaced by diaquahexacosaoxooctamolybdate(VI) ions and/or diaquapentacosaoxomonoperoxooctamolybdate(VI) ions (substitutional solid solution). The centrosymmetric [Mo 8 O 24 (O 2 ) 2 (H 2 O) 2 ] 4−  anion consists of six MoO 6  octahedra and two MoO 5 (O 2 ) pentagonal bipyramids, sharing edges. Selected bond distances: Mo–O peroxo  1.940(9) Å–1.964(10) Å, Mo=O terminal  1.681(6) Å–1.719(6) Å, Mo–O bridging  1.751(5) Å–2.429(5) Å and (O–O) peroxo  1.462(13) Å. Mo·· ·Mo edge–sharing  is 3.244(1) Å–3.494(1) Å and Mo…Mo corner–sharing  is 3.833(1) Å and 4.123(1) Å.

zeitschrift für kristallographie - crystalline materials

Studies on peroxomolybdates XXI. Crystal structure of the ammonium peroxooctamolybdate(VI) (NH 4 ) 4 [Mo 8 O 24+ x  (O 2 ) 2− x  (H 2 O) 2 ] · 4H 2 O ( x  = 0.8)  1