PROTONATION SITES IN A HETEROPOLYVANADATE OF PHOSPHORUS - X-RAY CRYSTAL-STRUCTURE OF (ME3NH)4(NH4)[H4PV14O42]

被引:61
作者
KHAN, MI
ZUBIETA, J
TOSCANO, P
机构
[1] SYRACUSE UNIV,CTR SCI & TECHNOL,DEPT CHEM,SYRACUSE,NY 13244
[2] SUNY ALBANY,DEPT CHEM,ALBANY,NY 12222
基金
美国国家科学基金会;
关键词
D O I
10.1016/S0020-1693(00)83792-5
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The reaction of (NH4)2HPO4 with (NH4)2Na2K2V10O28, followed by addition of Me3NHCl, yields dark crystals of the phosphovanadate cluster (Me3NH)4(NH4)[H4PV14O42]. The structure consists of an alpha-Keggin framework capped by two [VO] subunits. The protonation sites were identified as the doubly-bridging oxygens, O10. Crystal data: orthorhombic space group Fddd, a = 10.706(2), b = 23.581(4), c = 37.271(8) angstrom, V = 9409.3(22) angstrom3, Z = 8. X-ray data were collected on a Siemens R3m/V diffractometer using a theta/2-theta scan technique with graphite monochromated MoK-alpha radiation. A total of 2733 reflections was collected (to 2-theta = 55-degrees), of which 1850 were used in subsequent structure solution and refinement (I > 3-sigma(I)). The structure was solved by direct methods, and least-squares refinement converged at R = 0.033.
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页码:17 / 20
页数:4
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