Tungstorhenate heteropolyanions. 2. Synthesis and characterization of enneatungstorhenates(V), -(VI), and -(VII)
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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 P1̄; a = 10.194(1), b = 11.503(2), c = 9.682(1) Å; α = 100.55(1), β = 115.81(1), γ = 99.13(1)°; Z = 1], based on 3743 reflections, shows the anion to be isostructural with decatungstate, [W10O32]4-. Refinement in P1̄ 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.
Suggested Citation
Ortega, F., Pope, M., and Evans, H., 1997, Tungstorhenate heteropolyanions. 2. Synthesis and characterization of enneatungstorhenates(V), -(VI), and -(VII): Inorganic Chemistry, v. 36, no. 10, p. 2166-2169, https://doi.org/10.1021/ic961142q.
| Publication type | Article |
|---|---|
| Publication Subtype | Journal Article |
| Title | Tungstorhenate heteropolyanions. 2. Synthesis and characterization of enneatungstorhenates(V), -(VI), and -(VII) |
| Series title | Inorganic Chemistry |
| DOI | 10.1021/ic961142q |
| Volume | 36 |
| Issue | 10 |
| Publication Date | May 07, 1997 |
| Year Published | 1997 |
| Language | English |
| Publisher | American Chemical Society |
| Description | 4 p. |
| First page | 2166 |
| Last page | 2169 |