Hydrothermal Synthesis and Crystal Structure of a New Sandwich-type Molybdenum Phosphate

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The crystal structure of the title compound, [enH2][Fe{MoⅤ6O12(OH)3(HPO4)- (H2PO4)3}2]6en6H2O (en = H2NCH2CH2NH2), hydrothermally synthesized from a mixture of Na2MoO42H2O, Fe2(SO4)3, H3PO4, H2N(CH2)2NH2 and water, has been determined by single- crystal X-ray diffraction. The crystal is of triclinic, space group P?with a = 11.9014(1), b = 13.4246(2), c = 13.8719(2) , a = 87.465(1), b = 69.981(1), g = 64.960(1)? V = 1873.46(4) 3, Z = 1, Mr = 2997.89, F(000) = 1466, m = 2.427 mm-1 and Dc = 2.657 g/cm3. The final R = 0.0404 for 5570 observed reflections (I > 2s(I)). The structural analysis reveals that each cluster anion contains two coplanar {Mo6} rings of six edge-sharing Mo(O5OH) octahedra, and the two {Mo6} rings are linked together through one octahedral FeⅡ ion to generate a sandwich-type cluster with rigorous () symmetry. Moreover, these clusters are further linked into a three-dimensional frame- work by hydrogen bonds. The crystal structure of the title compound, [enH2] [Fe {MoV6O12 (OH) 3 (HPO4) - (H2PO4) 3} 2] 6en6H2O (en = H2NCH2CH2NH2), hydrothermally synthesized from a mixture of Na2MoO42H2O, Fe2 (SO4) , H3PO4, H2N (CH2) 2NH2 and water, has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P with a = 11.9014 (1), b = 13.4246 13.8719 (2) a = 87.465 (1) b = 69.981 (1) g = 64.960 (1) V = 1873.46 (4) 3 Z = 1 Mr = 2997.89 F (000) = 1466 m = 2.427 mm-1 and Dc = 2.657 g / cm3. The final R = 0.0404 for 5570 observed reflections (I> 2s (I)). The structural analysis reveals that each cluster anion contains two coplanar {Mo6} rings of six edge- sharing Mo (O5OH) octahedra, and the two {Mo6} rings are linked together through one octahedral FeIIion to generate a sandwich-type cluster with rigorous () symmetry. Moreover, these clusters are further linked into a three- by hydrogen bonds.
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