| Abstract: | The tungstorhenate(V) heteropolyanion [W9ReO32]5- has been isolated as guanidinium and cesium salts from reaction of [ReO2(PPh3)(py)3]+ with sodium tungstate. Crystallographic analysis of black Cs5[W9ReO32]??3H2O [triclinic, P1 or P1?? = 10.194(1), b = 11.503(2), c = 9.682(1) A??; a = 100.55(1), ??= 115.81(1), y = 99.13(1)??; Z = 1], based on 3743 reflections, shows the anion to be isostructural with decatungstate, [W10O32]4-. Refinement in P1 led to reliability indices R = 0.084, Rw = 0.046. Electrochemical investigation revealed the existence of ReVI and ReVII analogues, which were hydrolytically unstable in aqueous solution but which were isolated as crystalline tetra-n-butylammonium and tetra-n-heptylammonium salts, respectively, from nonaqueous solvents. The tetra-n-butylammonium salts of [W9ReVIO32]4- and [W10O32]4- were shown to be isomorphous by X-ray powder diffraction. Simulation of the Q-band ESR spectrum of [W9ReVIO32]4- (polycrystalline solid solution in [W10O32]4-) gave gx = 1.69(1), gy = 1.66(1), gz = 1.730(2) and 104Ax(185,187Re, I = 5/2) = (-)252(10), 104Ay = (-)398(10), 104Az = (-)653(5) cm-1. The orthorhombic ESR spectrum proves that the Re atom occupies one of the eight equivalent "equatorial" sites in the decatungstate structure. |
| Genre: | Article |
| ProdID: | 70019099 |
| Citation Author: | Ortega, F.; Pope, M. T.; Evans, Jr. , H. T. |
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| Citation End Page: | 2169 |
| Citation Issue: | 10 |
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| Citation Language: | English |
| Citation Larger Work Title: | Inorganic Chemistry |
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| Citation Number Of Pages: | 4 |
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| Citation Search Results Text: | Tungstorhenate Heteropolyanions. 2. Synthesis and Characterization of Enneatungstorhenates(V), -(VI), and -(VII); 1997; Article; Journal; Inorganic Chemistry; Ortega, F.; Pope, M. T.; Evans, Jr. , H. T. |
| Citation Start Page: | 2166 |
| Citation Volume: | 36 |
| Citation Year: | 1997 |
| Type: | citation/reference |
| Text: | Tungstorhenate Heteropolyanions. 2. Synthesis and Characterization of Enneatungstorhenates(V), -(VI), and -(VII); 1997; Article; Journal; Inorganic Chemistry; Ortega, F.; Pope, M. T.; Evans, Jr. , H. T. |
| URL (THUMBNAIL): | http://pubs.er.usgs.gov/thumbnails/outside_thumb.jpg |
| Date Other: | Wed, 1 Jan 1997 00:00 -0600 |
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