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Hydrothermal Synthesis and Structure of Two New Mo(V)-Oxide Phosphates
Authors:Wenbin Yang  Canzhong Lu  Chuande Wu  Shaofang Lu  Dingming Wu  Honghui Zhuang
Institution:(1) The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences, Fuzhou, Fujian, 350002, People's Republic of China
Abstract:Two new members of Mo(V) phosphates were synthesized by hydrothermal methods. (enH2)(enH)NaMo12O24(OH)6(HPO4)2(H2PO4)6]·(en)4·20H2O(1)(en=H2 NCH2CH2NH2)HAD-H2]2HAD-H]2Zn3Mo12O24(OH)6(PO4)2(HPO4)6]·6H2O (2) (HAD=H2N(CH2)6NH2). Compound 1 crystallized in the space group P2(1)/n, a=15.93120(10) Å, b=15.8946(2) Å, c=17.0665(2) Å, V=4316.02(8), beta=92.9060(10)°, Z=2. Compound 2 crystallized in the space group P(–1) with a=12.3726(3) Å, b=14.1948(3) Å, c=14.2310(4) Å, agr=72.7100(10), beta=65.0230(10), gamma=69.5600(10)°, Z=2089.70(9) Å3, and Z=1. The structure of 1 consists of sandwich-shaped cluster anion Na{MoV 6O12(OH)3(HPO4)(H2PO4)3}2]3– ({Na(Mo V 6 ) 2 }) held together via intermolecular hydrogen-bonding contacts. For the compound 2, the sandwich-shaped clusters ZnMo6O12(OH)3(PO4)(HPO4)3]2 ({Zn(Mo V 6 ) 2} are linked by tetrahedrally-coordinated zinc into layers. Organic cations (H3N(CH2)6NH3]2+ and H3N(CH2)6NH2]+) are filled in the spaces between lamellas. The layers are held together by a hydrogen-bonded network, which involves the terminal phosphate P-OH groups, as well as organic cations and several waters of solvation.
Keywords:hydrothermal synthesis  Mo(V)-oxide phosphates  crystal structures  hydrogen bonds
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