Synthesis and Crystal Structure of [H-amp]_4[Mo_8O_(26)(DMF)_2]·2H_2O (amp=2-Amino-6-methyl-pyridine

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The reaction of MoO2(acac)2 with 2-amino-6-methyl-pyridine (amp) in the mixed solvent of DMF (N,N-dimethylformamide) and water affords the title complex [H-amp]4- [Mo8O26(DMF)2]2H2O which was characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction analysis with the following crystallographic data: C30H54Mo8N10O30, Mr = 1802.35, monoclinic, P21/n, a = 8.631(1), b = 24.260(3), c = 13.351(2) ? b = 104.688(3), V = 2704.2(7) 3, Z = 2, Dc = 2.213 g/cm3, m =1.890 mm-1 and F(000) = 1760. The final R = 0.0281 and wR = 0.0620 for 4935 observed reflections with I > 2s(I). X-ray structure analysis has confirmed the existence of g-[Mo8O26]4- anion in the molecule. Eight MoO6 distorted octahedra share edges with short terminal MoO bonds from 1.691(3) to 1.749(2) ? medium bonds from 1.868(2) to 1.965(2) ?and long bonds from 2.059(2) to 2.450(2) ? In the terminal site there exist two DMF ligands bound to the Mo atom through O atoms with the MoODMF bond length of 2.166(3) ? affording a bond strength of 0.433. A three-dimensional network structure was formed through hydrogen bonds. The reaction of MoO2 (acac) 2 with 2-amino-6-methyl-pyridine in the mixed solvent of DMF (N, N-dimethylformamide) and water affords the title complex [H- amp] 4- [Mo8O26 DMF) 2] 2H2O which was characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction analysis with the following crystallographic data: C30H54Mo8N10O30, Mr = 1802.35, monoclinic, P21 / n, a = 8.631 (1), b = 24.260 (3) c = 13.351 (2)? B = 104.688 (3) V = 2704.2 (7) 3 Z = 2 Dc = 2.213 g / cm3 m = 1.890 mm-1 and F 1760. The final R = 0.0281 and wR = 0.0620 for 4935 observed reflections with I> 2s (I). X-ray structure analysis has confirmed the existence of g- [Mo8O26] 4-anion in the molecule. Eight MoO6 distorted octahedra share edges with short terminals MoO bonds from 1.691 (3) to 1.749 (2)? medium bonds from 1.868 (2) to 1.965 (2)? and long bonds from 2.059 (2) to 2.450 (2)? In the terminal site exist two DMF ligands bound to the Mo atom through O atoms with the MoODMF bond length of 2.166 (3)? Affording a bond strength of 0.433. A three-dimensional network structure was formed through hydrogen bonds.
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