A Nickel Molybdenum Phosphate with Tunnel: Hydrothermal Synthesis and Structure of (NH3CH2CH2NH3)4 · (NH3CH2CH2NH2) · Na · [Ni2Mo12O30(PO4)(HPO4)4(H2PO4)3] · 6H2O

✍ Scribed by Lin Xu; Yaqiu Sun; Enbo Wang; Enhong Shen; Zhongri Liu; Changwen Hu; Yan Xing; Yonghua Lin; Hengqing Jia

• Publisher: Elsevier Science
• Year: 1999
• Tongue: English
• Weight: 158 KB
• Volume: 146
• Category: Article
• ISSN: 0022-4596
• DOI: 10.1006/jssc.1999.8368

✦ Synopsis

A nickel molybdenum phosphate, (NH 3 CH 2 CH 2 NH 3 ) 4 ' (NH 3 CH 2 CH 2 NH 2 ) ' Na ' [Ni 2 Mo 12 O 30 (PO 4 ) (HPO 4 ) 4 (H 2 PO 4 ) 3 ] ' 6H 2 O, involving molybdenum present in V oxidation, has been hydrothermally synthesized and structurally characterized by single crystal X-ray di4raction. Deep brown-red crystals are formed in the triclinic system, space group P1 , a ‫؍‬ 12.011(2), b ‫؍‬ 14.612(3), c ‫؍‬ 21.252(4) A s , ‫؍‬ 80.54(2)3, ‫؍‬ 83.10(2)3, ‫؍‬ 76.29(2)3, V ‫؍‬ 3561.4(12) A s 3 , Z ‫؍‬ 2, (MoK ) ‫؍‬ 0.71073 A s (R(F) ‫؍‬ 0.0529 for 9880 re6ections). Data were collected on a Siemens P4 di4ractometer at 203C in the range of 1.753 < < 23.023 using the -scan technique. The structure was solved by direct methods using the program SHELXTL-93 and re5ned with the method of full-matrix least-squares on F 2 . The structure of the title compound may be considered to be two [Mo 6 O 15 (HPO 4 )(H 2 PO 4 ) 3 ] 5؊ units bonded together with a nickel atom, although several P+O groups are not protonated on account of coordination with a Na ؉ cation. The one-dimensional tunnels were formed in the solid of the title compound. A probe reaction of the oxidation of acetaldehyde with H 2 O 2 using the title compound as catalyst was carried out in a liquid+ solid system, showing that the title compound had high catalytic activity in the reaction.