The Crystal Structure of Potassium Nickel(IV) Hexaoxidoiodate(VII).

Eddy, Lowell P.; Vannerberg, Nils-Gösta; Kemp, E; Møller, Jørgen; Sjöberg, Berndt; Bunnenberg, E.; Djerassi, Carl; Records, Ruth

doi:10.3891/acta.chem.scand.20-2886

Cited by 15 publications

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“…An value of roughly 0.73, with only a weak dependence on the k -weighting exponent, was obtained. The quality of the single-shell fit was improved when a theoretical standard generated using more recent structure data for KNiIO 6 (refs and ) was used. The more recent X-ray diffraction structure data give a Ni−O distance of 1.80 Å, which is closer to the true distance than the 2.18 Å distance obtained from earlier results (Table ).…”

Section: Resultsmentioning

confidence: 99%

“…SSR: sum of the square of residuals between experimental and calculated spectra. Fits were performed using theoretical standards generated from structure data for NiO (model M1), β-Ni(OH) 2 (model M2), and KNiIO 6 with structure data from ref (model M4) or refs and (model M5). All fits were refined over the k -range 4−14 Å -1 .…”

Section: Resultsmentioning

confidence: 99%

“…To aid in the analysis of XAS data, nickel local structure parameters as well as lattice type, space group, and unit cell dimensions are listed in Table for Ni, NiO, β-Ni(OD) 2 and β-Ni(OH) 2 based on neutron diffraction data and XRD data, α-Ni(OH) 2 , LiNiO 2 , , and KNiIO 6 . , Structural parameters for KNiIO 6 based on more recent XRD data were also included . The XRD data for LiNiO 2 are consistent with neutron diffraction data for an Li 0.4 Ni 0.6 O sample which is closely related in composition with our sample except for a difference in the position of the oxygen atoms .…”

Section: Methodsmentioning

confidence: 99%

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Analysis of X-ray Absorption Spectra of Some Nickel Oxycompounds Using Theoretical Standards

1998

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X-ray absorption spectra have been measured for NiO, β-Ni(OH) 2 , R-Ni(OH) 2 , LiNiO 2 , and KNiIO 6 samples, which contain nickel with valency in the range 2-4. Information on the local structure and nature of bonding of nickel compounds has been derived using theoretical standards generated with the FEFF code. The Ni K-edge energy was found to shift to higher values by about 1.5 eV per unit change in valency of nickel. The energy of the preedge peak (generally attributed to the transition from the 1s core states to the 3d unoccupied states) shifts to higher values by about 0.6 eV per unit change in valency of nickel. A many body amplitude reduction factor (S 0 2 ) of 0.77 ( 0.03 for Ni K-edge absorption can be used to scale theoretical spectra to fit the experimental ones in order to accurately determine the coordination numbers for compounds with complex structures. Our results show that chemical effects are very small and can be ignored for reliable structural analysis. Results of local structure for the first, second, and third coordination spheres for NiO are consistent with those derived from X-ray diffraction data. The results for β-Ni(OH) 2 are much closer in agreement with those derived from the neutron diffraction data rather than the X-ray diffraction data. The results for R-Ni(OH) 2 differ significantly from those based on the idealized structure model proposed by Bode et al. In fact, the structure within the hexagonal planes for R-Ni(OH) 2 is similar to that for β-Ni(OH) 2 . The apparent contraction in the Ni-Ni distance of the third coordination sphere for R-Ni(OH) 2 relative to that for β-Ni-(OH) 2 , which was previously reported by others, is not real and can be attributed to structural disorder. The Ni-O bond length for divalent nickel with an octahedral coordination is in the range 2.06-2.08 Å. The first coordination sphere for LiNiO 2 consists of four and two oxygens at 1.91 and 2.06 Å, respectively, rather than six oxygens at 2.04 Å, as predicted by the X-ray diffraction data. The short distance is characteristic of Ni 3+ -O 2bonds and Ni 2+ -O -bonds, while the long distance is characteristic of Ni 2+ -O 2bonds. The local structure for LiNiO 2 is consistent with the fact that the charge-compensating mechanism is largely due to oxygen 2p holes. The Ni-Ni second-shell distance for LiNiO 2 is consistent with that based on the X-ray and neutron diffraction data. The Ni-O bond length for quadrivalent Ni in KNiIO 6 is 1.88 Å. The Ni-O bond length varies with nickel valency in a nonlinear manner.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

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Analysis of X-ray Absorption Spectra of Some Nickel Oxycompounds Using Theoretical Standards

1998

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“…Although Sn and Te have very similar scattering factors for both X-rays and neutrons, their ordering in the starting Na2SnTeO6 is 19 (c) disordered stacking, i.e., random intergrowth of structures (a) and (b), that should be described as rosiaite aristotype, P3 � 1m, with mixed Sn0.5Te0.5 occupancy on Sb sites. Due to similarity of scattering factors for Sn and Te, no considerable superlattice reflections can be expected in model (a), whereas models (b) and (c) do not generate superlattice reflections at all.…”

Section: 2crystal Structurementioning

confidence: 99%

Trigonal layered rosiaite-related antiferromagnet MnSnTeO₆: ion-exchange preparation, structure and magnetic properties

et al. 2018

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“…A variety of compounds containing orthoperiodate [IO 6 ] 5− anions and alkali metal cations were reported. Their structures include isolated [IO 6 ] 5− anions, e. g. in K 6 Na(AuO 2 )(IO 6 ), [17] metal complexes, e. g. [(IO 6 ) 2 (MoO 2 ) 2 ] 6− in K 6 [(IO 6 ) 2 (MoO 2 ) 2 ] ⋅ 10H 2 O, [18] layers, e. g.

_{\infty}^{2} [{normalM (IO}_{6}) {]​}^{3 - -}

honeycombs in A [Ni(IO 6 )] ( A =Na, K) [19,20] and Rb[ M (IO 6 )] ( M =Ge, Sn, Pb), [21] or three‐dimensional frameworks, e. g. in the double‐perovskites AE Na(IO 6 ) ( AE =Ca, Sr, Ba, Pb) [22–24] . The here reported compound K 8 [Rh(IO 6 ) 2 ]OH ⋅ 3H 2 O represents the first rhodium periodate [25,26] …”

Section: Introductionmentioning

confidence: 99%

Orthoperiodato Rhodium(III) Complex as a Possible Key to Catalytic Oxidation of Organic Dyes

Albrecht

Ruck

2022

Zeitschrift anorg allge chemie

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Dedicated to Professor Mercouri Kanatzidis on the Occasion of his 65 th Birthday.Light yellow, air-sensitive single-crystals of the rhodium(III) orthoperiodato K 8 [Rh(IO 6 ) 2 ]OH • 3H 2 O were synthesized starting from Rh 2 O 3 and KIO 4 . The reaction was carried out in a potassium hydroxide hydroflux with a molar water-base ratio of 1.8 at 200 °C. Single-crystal X-ray diffraction revealed a triclinic crystal structure (space group P1). The most striking feature of the structure is the [Rh(IO 6 ) 2 ] 7À anion, a linear sequence of three face-sharing octahedra. It can be interpreted as a rhodium(III) cation coordinated by two orthoperiodato groups. A water molecule and a hydroxide ion form an associate (H 3 O 2 ) À . Together with other water molecules, they connect the [Rh-(IO 6 ) 2 ] 7À anions via hydrogen bridges to form layers. Upon heating, the compound first loses its crystal water, then the iodine is gradually reduced before evaporating during the final decomposition step, which results in K 0.63 RhO 2 . In K 8 ) 2 ]OH • 3H 2 O, the unusually short Rh III À I VII distance of only 276.38(1) pm should allow direct charge transfer in the [Rh(IO 6 ) 2 ] 7À anion. An electron-poor rhodium cation, accessible from the side, could be the active center in the rhodiumcatalyzed oxidation of unsaturated organic molecules by periodate.

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The Crystal Structure of Potassium Nickel(IV) Hexaoxidoiodate(VII).

Cited by 15 publications

References 0 publications

Analysis of X-ray Absorption Spectra of Some Nickel Oxycompounds Using Theoretical Standards

Analysis of X-ray Absorption Spectra of Some Nickel Oxycompounds Using Theoretical Standards

Trigonal layered rosiaite-related antiferromagnet MnSnTeO₆: ion-exchange preparation, structure and magnetic properties

Orthoperiodato Rhodium(III) Complex as a Possible Key to Catalytic Oxidation of Organic Dyes

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The Crystal Structure of Potassium Nickel(IV) Hexaoxidoiodate(VII).

Cited by 15 publications

References 0 publications

Analysis of X-ray Absorption Spectra of Some Nickel Oxycompounds Using Theoretical Standards

Analysis of X-ray Absorption Spectra of Some Nickel Oxycompounds Using Theoretical Standards

Trigonal layered rosiaite-related antiferromagnet MnSnTeO6: ion-exchange preparation, structure and magnetic properties

Orthoperiodato Rhodium(III) Complex as a Possible Key to Catalytic Oxidation of Organic Dyes

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Trigonal layered rosiaite-related antiferromagnet MnSnTeO₆: ion-exchange preparation, structure and magnetic properties