Synthesis,spectroscopic and structural studies of tris(3-methyl-pyridinium)(3-ethylpyridinium)β-octamolybdate monohydrate |
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Authors: | Pascual Román Juan M Gutiérrez-Zorrilla Martín Martínez-Ripoll Severino García-Blanco |
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Institution: | (1) Departamento de Química Inorgánica, Universidad del País Vasco, Apartado 644, 48080 Bilbao, Spain;(2) U.E.I. de Cristalografía, Instituto Rocasolano, C.S.I.C., Serrano 119, 28006 Madrid, Spain |
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Abstract: | Summary Three isostructural compounds of general formula (3-MepyH)
x
(3-EtpyH)4–x
Mo8O26] (x=0, 2, 4) crystallize in the monoclinic system, space group P21/n, Z=2. Previously determined parameters for the compoundx=4 area=13.652(2),b=10.887(1),c=13.759(1) Å, =90.87(1)°,V=2044.8(4) Å3,Dx=2.53,Do=2.54(1) mg m–3,F(000)=1496. Slight differences in cell dimensions have been observed whenx=0 or 2. A nonisomorphous compound of formula (3-MepyH)3(3-EtpyH)Mo8O26]·H2O crystallizes in the triclinic system, space group P21/n,Z=2,a=10.918(1),b=10.985(3),c=18.991(2) Å, =97.19(2), =91.45(2), =107.30(2)0,V=2152.8(7) Å3,Dx=2.456,Do=2.456(5) mg m–3,F(000)=1532. The distinguishing features of tris(3-methylpyridinium)(3-ethylpyridinium) -octamolybdate monohydrate are its non-centrosymmetric polyanion and its extensive hydrogen bonding. The asymmetric unit contains three independent 3-methylpyridinium and one 3-ethylpyridinium cations, one water molecule and the -octamolybdate anion. The planar cations are oriented to permit hydrogen bonds with either molybdate oxygen atoms or water oxygen atoms. Four different types of hydrogen bonds have been found: N–H...O (mono- and bifurcated); N–H...Ow (monofurcated); Ow–Hw...O (monofurcated); and C–H...O (monofurcated). The proposed hydrogen bonding interactions appear to stabilize the structure. |
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