Refinement of Ammonium Perrhenate Structure Using a Pseudo-Spin Model for the Ammonium Ion Orientation
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A new Rietveld refinement of previously reported powder neutron diffraction data on ND 4 ReO 4 taken over a wide range of temperatures [Powell, Brown, Harnden & Reid (1993). Acta Cryst . B 49 , 463–468] is reported. Rigid-body constraints are applied to the cation geometry and occupation of a second cation orientation at higher temperatures is permitted. The resulting structure at higher temperatures is to be preferred to the previous structure with a single cation orientation and supports the pseudo-spin theory of cooperative disordering without a phase transition.Keywords:
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Rietveld Refinement
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Tetrapyridinesilver(I) perrhenate [Agpy4]ReO4 was synthesized, and its crystal structure and Raman spectra were elucidated at low temperatures. The crystal lattice is constructed from isolated tetrahedral cations and anions having no argentophilic interactions. Weak hydrogen bonds are formed between the oxygens of the disordered perrhenate anions and the ortho-hydrogens of the pyridine ligands. No parallel π…π stacking interactions are observed, but C-H…π interactions of the pyridine ligands within columns of cations and between the columns appeared. Correlation analysis for Ag+, pyridine ligands, and perrhenate ions was performed, and the perrhenate ion and some of the AgN4 skeleton vibrational modes and pyridine ligand modes in the Raman spectrum of [Agpy4]ReO4 were assigned.
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The photoelectron spectroscopic binding energies of Se 3d5/2, O 1s, and Cl 2p3/2 or Re 4f7/2 have been measured in tetralmethyltetraselenafulvalenium (TMTSF) perchlorate and perrhenate, tetrabutylammonium perchlorate and perrhenate, and potassium perchlorate and perrhenate. It has been found that the binding energies of Se 3d5/2 are the same in the perchlorate and the perrhenate even though the spectrum is more asymmetrically broadened in the perrhenate. The binding energy of O 1s depends on the cation and on the central atom in the anion. In the organic perrhenates it is at 530.96 eV, whereas in the perchlorates it is at 532.08 eV. In the potassium salts the O 1s binding energies differ by 1.89 eV in the perchlorate and the perrhenate. The binding energies of Cl 2p3/2 and Re 4f7/2 differ by 0.84 and zero respectively from those in the potassium salts. The energetic differences among the values for O 1s indicate the extent to which the electronic structure of the TMTSF salts are determined by the electronic structure of the anions. The difference in binding energies between the TMTSF perchlorate and perrhenate is such that the application of pressure to the perrhenate should transfer electrons to the cation and presumably to the conduction band.
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Abstract Brilliant green perrhenate has been applied in a liquid-state ion-selective electrode for the determination of perrhenate. Near Nernstian response is obtained in the range 10−5 − 10−2 M perrhenate, and the response is independent of pH in the pH range 5.0 − 7.2.
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Gravimetric analysis
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Ethyltriphenylphosphonium perrhenate, (C20H20P)[ReO4], and (iodomethyl)triphenylphosphonium perrhenate, (C19H17IP)[ReO4], have been crystallized from 2-propanol. Both crystal structures consist of phosphonium cations and perrhenate anions. The cations show the typical propeller-like geometry. In both crystals, the positions of the nearly tetrahedral anions are stabilized by weak C—H⋯O hydrogen bonds, and for the latter compound, I⋯π interactions also occur.
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