Studies on peroxomolybdates XXI. Crystal structure of the ammonium peroxooctamolybdate(VI) (NH4)4[Mo8O24+x(O2)2−x(H2O)2] · 4H2O (x = 0.8)1
Abstract
The crystal structure of (NH4)4 · [Mo8O24+x(O2)2−x(H2O)2] · 4H2O (x = 0.8) has been determined from single-crystal X-ray diffraction data. The yellow compound crystallizes in the monoclinic space group P21/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) Å3 and Z = 2. Full-matrix least-squares refinement of 213 structural parameters gave R(F) = 0.034 (Rw(F) = 0.042) for 2630 observed [I > 3σ(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 The formula implies that part of the diaquatetracosaoxodiperoxooctamolybdate(VI) ions have been replaced by diaquahexacosaoxooctamolybdate(VI) ions and/or diaquapentacosaoxomonoperoxooctamolybdate(VI) ions (substitutional solid solution).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 [Mo8O24(O2)2(H2O)2]4− anion consists of six MoO6 octahedra and two MoO5(O2) pentagonal bipyramids, sharing edges. Selected bond distances: Mo–Operoxo 1.940(9) Å–1.964(10) Å, Mo=Oterminal 1.681(6) Å–1.719(6) Å, Mo–Obridging 1.751(5) Å–2.429(5) Å and (O–O)peroxo 1.462(13) Å. Mo·· ·Moedge–sharing is 3.244(1) Å–3.494(1) Å and Mo…Mocorner–sharing is 3.833(1) Å and 4.123(1) Å.
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Articles in the same Issue
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- Kinetic and microstructural studies of the crystallisation of coesite from quartz at high pressure
- Studies on peroxomolybdates XXI. Crystal structure of the ammonium peroxooctamolybdate(VI) (NH4)4[Mo8O24+x(O2)2−x(H2O)2] · 4H2O (x = 0.8)1
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