Abstract:Synchrotron X-ray powder diffraction data (SPDD) for representative LiMF6 and Li2MF6 salts of the second and third transition series have provided unit-cell parameters and, from Rietveld analysis, M-F interatomic distances. M-F distances have also been obtained from X-ray single-crystal structural analyses of LiOsF6, Li2PtF6, and KRhF6. The LiMF6 all have the LiSbF6 structure type (space group R3). For M = Ta to Au the primitive unit cell volume decreases with increasing nuclear charge (Z), the volumes (sigma … Show more
“…[1,2] Further stabilization of Pd IV is achieved by formation of [PdF 6 ] 2À complexes which exist for many counter cations. [3] A limited number of such complex anions is also known for other halides, and the palladates A 2 [PdX 6 ] (A= alkaline metal; X = Cl, Br, I) are stable compounds, even if the binary halides PdX 4 (X = Cl, Br, I) cannot be obtained. [4] Oxygen should also be a suitable oxidant for the preparation of tetravalent palladium compounds and, indeed, a number of complex oxides are known which have been obtained in most cases from high-pressure reactions.…”
For the first time tetravalent palladium is detected, coordinated exclusively by simple oxoanions. Stabilization was achieved by formation of the [Pd(S2 O7 )3 ](2-) complex in which three chelating disulfate groups surround the metal atom. The salt K2 [Pd(S2 O7 )3 ] could only be obtained if the reaction of K2 [PdCl6 ] and neat SO3 was performed in the presence of XeF2 .
“…[1,2] Further stabilization of Pd IV is achieved by formation of [PdF 6 ] 2À complexes which exist for many counter cations. [3] A limited number of such complex anions is also known for other halides, and the palladates A 2 [PdX 6 ] (A= alkaline metal; X = Cl, Br, I) are stable compounds, even if the binary halides PdX 4 (X = Cl, Br, I) cannot be obtained. [4] Oxygen should also be a suitable oxidant for the preparation of tetravalent palladium compounds and, indeed, a number of complex oxides are known which have been obtained in most cases from high-pressure reactions.…”
For the first time tetravalent palladium is detected, coordinated exclusively by simple oxoanions. Stabilization was achieved by formation of the [Pd(S2 O7 )3 ](2-) complex in which three chelating disulfate groups surround the metal atom. The salt K2 [Pd(S2 O7 )3 ] could only be obtained if the reaction of K2 [PdCl6 ] and neat SO3 was performed in the presence of XeF2 .
“…The generation of the red gas PtF 6 by room temperature oxidation with cationic Ag III (possibly AgF 2(aHF) + ), was achieved in greater than 70% yield: Ag ðaHFÞ 3þ þ PtF 6ðaHFÞ À ! Ag ðaHFÞ 2þ þ PtF 6ðgÞ (10) Although neither this oxidizer nor cationic Ni IV was able to liberate AuF 6 from its monoanion [29], we can be sure that these reagents are the most potent oxidizers yet made. Hitherto, KrF + has had that distinction [30], but as Gillespie and Schrobilgen found [31], the compound KrFPtF 6 does not release PtF 6 , but decomposes with loss of Kr, and F 2 , and formation of PtF 5 .…”
Section: Cationic Ag III and Ni Iv -Oxidizers Par Excellencementioning
“…The first compounds containing these species were prepared by Hepworth and coworkers [1]: MOsF 6 (M = Li, K, Rb, Cs, Ag) and M 2 OsF 6 (M = K, Cs), and were later characterized by various techniques, such as IR spectroscopy [2][3][4][5][6] and X-ray diffraction [7][8][9]. Both anions can be of relevance for the urban mining processes [10,11] and the analytical chemistry of osmium [12,13].…”
Two barium hexafluoridoosmates, Ba(OsF 6 ) 2 and BaOsF 6 , were synthesized and were characterized for the first time using X-ray powder and single crystal diffraction, IR spectroscopy, as well as NMR spectroscopy in anhydrous hydrogen fluoride. Ba(OsF 6 ) 2 crystallizes in the space group type P2 1 /c with the cell parameters a = 6.4599 (4)
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